CN109234769A - A kind of preparation method of ultra-thin metal layer - Google Patents
A kind of preparation method of ultra-thin metal layer Download PDFInfo
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- CN109234769A CN109234769A CN201811172751.6A CN201811172751A CN109234769A CN 109234769 A CN109234769 A CN 109234769A CN 201811172751 A CN201811172751 A CN 201811172751A CN 109234769 A CN109234769 A CN 109234769A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 103
- 239000002184 metal Substances 0.000 title claims abstract description 102
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 238000005323 electroforming Methods 0.000 claims abstract description 131
- 239000011159 matrix material Substances 0.000 claims abstract description 24
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 22
- 238000004070 electrodeposition Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000004062 sedimentation Methods 0.000 claims abstract description 10
- 230000001052 transient effect Effects 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 59
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 32
- 229910052802 copper Inorganic materials 0.000 claims description 32
- 239000010949 copper Substances 0.000 claims description 32
- 238000000151 deposition Methods 0.000 claims description 15
- 230000008021 deposition Effects 0.000 claims description 13
- 230000005611 electricity Effects 0.000 claims description 12
- 238000010899 nucleation Methods 0.000 claims description 12
- 230000006911 nucleation Effects 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000000970 chrono-amperometry Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 238000004832 voltammetry Methods 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims 2
- 229910001338 liquidmetal Inorganic materials 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 5
- 238000013329 compounding Methods 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 238000010586 diagram Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
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- 238000000280 densification Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/10—Moulds; Masks; Masterforms
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
Abstract
The present invention relates to electroforming process technical fields, a kind of preparation method of ultra-thin metal layer is provided, the preparation method of the ultra-thin metal layer prepares ultra-thin metal layer by electro-deposition method on matrix, pass through compounding high concentration electroforming solution, to guarantee that metal ion transient state is nucleated, meanwhile, it is controlled in conjunction with current density, so that operating potential is more than the sedimentation potential of metal ion, guarantee that matrix surface forms the ultra-thin metal layer less than 1 micron.
Description
Technical field
The present invention relates to electroforming process technical field, in particular to a kind of preparation method of ultra-thin metal layer.
Background technique
Currently, present electronic product is to increasingly minimizing, the development of components densification interconnects the copper of its wiring board
Technique also proposed more and more thinner and accurate requirement.Metal layer preparation be accuracy electroplate, the relevant integrated circuit of precise electrotyping,
The technological means being usually related in each technical fields such as electronic component manufacturing technology field, mold galvanoplastics field, still
How thickness ultrathin effectively is made, the smooth fine metal layer in surface is metal layer preparation method technical problem urgently to be solved.
In addition, electroforming refers to the electro-deposition on core model, then separate with the technique of manufacture (or duplication) metal product.Electroforming
Deposited metal, alloy or composite material on conductive former mould (master mold) using metal ion negative electrode electro-deposition principle, and by its
It is separated with former mould to produce the process of product.Usually conductive former mould makees cathode, needs the metal of electroforming to make anode, is put into electricity together
It casts in solution, passes to direct current, electroforming solution is the solution containing anode metal ion, under the action of power supply, electroforming solution
In metal ion be reduced into metal on the conductive former mould of cathode, be deposited on conductive master surface, meanwhile, anode metal is in a steady stream not
Become ion-solubility disconnectedly to be supplemented into electroforming solution, remains unchanged the concentration of metal ion in electroforming solution.When cathode is led
Electroformed layer on electric former mould gradually increases, and when reaching requirement thickness, stops electroforming, and electroforming part is separated with former mould, is obtained and original
The opposite electroforming part in model face.The shape and surface roughness value of this electroforming part are similar to former mould.It can be tired machining
Difficult inner surface is converted into master mold outer surface, can accurately replicated surfaces profile and fine lines, can obtain dimensional accuracy it is high,
The good product of surface smoothness, thus it is used to manufacture hollow parts complex-shaped, with high accuracy, injection molding mold, duplication
Fine surface profile etc..But under the conditions of conventional electroforming process, electroforming part can only obtain rougher surface, and
When carrying out the separation of electroforming part, it is easy due to the excessive demoulding of electroformed layer and the too small demoulding of conductive former mould (master mold) binding force, binding force
The case where generating separation tearing, conductive original mould (master mold) surface are destroyed, and conductive original mould (master mold) can be replicated number reduction, lead
Electric original mould (master mold) utilization rate is low.And the electric casting die much obtained at present by electroforming, especially with the light of micro-structure
Learn mold, it is desirable that surface roughness is extremely low (tens or even several nanometers), and its conductive former mould (master mold) master tooling cost is high,
Cost of manufacture is considerably increased, is not suitable for quantitatively producing and using, this just proposes very high requirement to precise electrotyping.
Summary of the invention
Therefore, for above-mentioned problem, the present invention proposes a kind of preparation method of ultra-thin metal layer, passes through electro-deposition method
Ultra-thin metal layer is prepared on matrix, by compounding high concentration electroforming solution, to guarantee that metal ion transient state on matrix is nucleated, together
When, it is controlled in conjunction with current density, so that operating potential is more than the sedimentation potential of metal ion, guarantees that matrix surface forms ultra-thin gold
Belong to layer.
To realize above-mentioned technical problem, the solution that the present invention takes are as follows: a kind of preparation method of ultra-thin metal layer, packet
Include following steps:
Step 1 prepares electroforming solution, and electroforming solution is that the metal salt containing the metal ion for constituting ultra-thin metal layer is molten
Liquid；Electroforming solution is high concentration electroforming solution, its metal ion is on matrix with transient state nucleation side when high concentration electroforming solution is for electroforming
Formula is reduced；
Step 2, the acetone soak oil removing of the matrix of depositing ultrathin metal layer is needed, then successively with dehydrated alcohol, super
Pure water is cleaned by ultrasonic 15-25 minutes；The metal plate for constituting ultra-thin metal layer with nitric acid dousing 10-15 seconds, then successively
It carries out ultrapure water, be dried with nitrogen；
Matrix is immersed in electroforming solution by step 3 together as cathode, metal plate as anode, is led between cathode, anode
Electricity carries out current density adjusting, and power supply can show that corresponding operating potential, control operating potential are higher than electricity when current density is adjusted
The sedimentation equilibrium current potential of the metal ion of liquid is cast, while controlling operating potential lower than current potential is limited, limiting current potential is to guarantee electroforming
The metal ion of liquid not will form the current potential upper limit of sand-like particle deposition, carry out electro-deposition 0.5-40 seconds, in the surface shape of matrix
At there is ultra-thin metal layer, matrix is then taken out, with the abundant rinsing, drying of deionized water, the ultra-thin metal layer preparation is completed.
Further, the concentration of step 1 middle and high concentration electroforming solution is determined using chronoamperometry: passing through chronoamperometry
The electroforming solution of various concentration is tested, the relation curve of the electric current i and response time t of the electroforming solution of each concentration are obtained,
That is current versus time curve obtains corresponding Limited diffusion current density according to the current versus time curve of the electroforming solution of each concentration
im, time t used in the diffusion current density that reaches capacitym, to obtain the zero dimension of the electroforming solution of each concentrationRelationship
Curve, by the zero dimension of the electroforming solution of each concentrationRelation curve and the zero dimension for judging nucleation mode
Theoretical curve (S-H curve) compares, when the zero dimension of electroforming solutionThe nothing that relation curve becomes together in instantaneous nucleation
DimensionWhen theoretical curve, judge the electroforming solution of its corresponding concentration metal ion can transient state nucleation, that is, determine energy
The concentration of the high concentration electroforming solution of enough transient state nucleation.
Further, the metal ion deposition equilibrium potential of electroforming solution is determined using voltammetry in step 3, work as volt
Cathode current curve is when there is electric current loop in the volt-ampere curve that peace method is presented, corresponding to current potential, that is, electroforming solution metal
Sedimentation equilibrium current potential.
It is determined further, limiting current potential in step 3 and continuously adjusting method using current density, current density is adjusted
When power supply can show corresponding operating potential, then it is constantly continuous improve current density, while observing the metal ion of electroforming solution
Sedimentation state, when there is sand-like particle deposition, corresponding operating potential limits current potential.
Further, carrying out ultrasonic vibration to the matrix as cathode in step 3, ultrasonic vibration frequency is 20-
1000KHz.The uniformity of deposited particles on matrix surface is able to ascend by ultrasonic vibration.
Further, using pulse current in step 3, the duty ratio of pulse current is 20%-55%.Pass through pulse
Electric current can promote the surface smoothness of ultra-thin metal layer.
Further, it is 0.5-2 seconds that control, which carries out electrodeposition time, in step 3.Strict control electrodeposition time, with
The preparation of ultra-thin metal layer is rapidly completed in short time, ultra-thin metal layer obtained is ultra-thin ultra dense discontinuous deposition layer, should
Under the conditions of ultra-thin metal layer can be used as the intermediate metal (electroformed deposit face) of electroforming master tooling, to solve existing electricity
It casts master tooling to be used for high existing surface roughness when electroforming, demoulding difficulty, the problem of demoulding tearing phenomenon occur, to improve electricity
Cast the accuracy of repetition and number of copy times of master tooling.
Further, described matrix is copper electroforming master tooling；The copper electroforming master tooling is in use, ultra-thin metal layer is used
Do electroformed deposit face.
Further, it is 10-40 seconds that control, which carries out electrodeposition time, in step 3.Strict control electrodeposition time, with
The preparation of ultra-thin metal layer is completed in long-time electro-deposition, and ultra-thin metal layer obtained is ultra-thin ultra dense continuous electro-deposition layer, this
Ultra-thin metal layer under part can be used in the metal layer of integrated circuit, electronic component manufacturing technology field, have nano thickness,
The small feature of continuous conduction, resistance.
Further, described matrix is integrated circuit board, the ultra-thin metal layer is used as conductive path.
Further, the ultra-thin metal layer is lead layer, the concentration of electroforming solution is 6~10mmol/L, current density 5
~8.5A/dm2。
Further, the ultra-thin metal layer is zinc layers, the concentration of electroforming solution is 0.5~2mol/L, and current density is
10~15.5A/dm2。
Further, the ultra-thin metal layer with a thickness of less than 1 μm.
By using preceding solution, the beneficial effects of the present invention are: the system of the ultra-thin metal layer designed as described above
Preparation Method is carried out the preparation of ultra-thin metal layer using electrodeposition process, ultra-thin metal layer can be made in various fine labyrinths
Matrix surface on uniform deposition, meanwhile, by electroforming solution concentration, current density, ultrasonic vibration frequency, electrodeposition time etc.
The adjusting of parameter can be realized the adjusting of ultra-thin metal layer nucleation closeness, convenient for controlling the grain density of ultra-thin metal layer；It should
Pass through compounding high concentration electroforming solution during preparation method, to guarantee that metal ion transient state is nucleated, meanwhile, in conjunction with current density control
System can guarantee that matrix surface forms ultra-thin gold of the thickness less than 1 micron so that current density is more than the sedimentation potential of metal ion
Belong to layer, i.e. nano-scale crystal nucleation layer.
In addition, the preparation method according to the ultra-thin metal layer carries out ultra-thin metal layer deposition, electricity in electroforming master tooling
When casting master mold and being made for electroforming part, interface in the combination of ultra-thin metal layer, that is, between electroforming master mold and electroforming part, super thin metal
Layer is ultra-thin ultra dense discontinuous deposition layer, then is noncontinuity faying face between electroforming master mold and electroforming part, meanwhile, pass through control
The grain density of ultra-thin metal layer processed can control the noncontinuity density combined between electroforming master mold and electroforming part, adjust two
Noncontinuity bonded area between person, then when carrying out the duplication of electroforming part using the electroforming master tooling, very thin super thin metal
Layer can adjust the binding force between electroforming master tooling and electroforming part, not only can be reduced the residual stress on electroforming master tooling surface, but also
It can be reduced electroforming master tooling surface roughness, and the demoulding of electroforming part is very laborsaving, hence it is evident that reduce separation tearing phenomenon, protection is female
Mold reduces electric surface roughness, and therefore, the electroforming master tooling electro-deposition accuracy of repetition for being deposited with ultra-thin metal layer is excellent
Different, number of copy times is promoted, and the electro-deposition suitable for high-precision mold replicates, especially with the optical mould of micro-structure, preparation
Method is simple, and preparation cost is low, is suitble to quantitatively promote the use of, practicability is high.
Detailed description of the invention
Fig. 1 is roughness comparison diagram.
The copper electroforming master tooling and the state diagram after the demoulding of the nickel part obtained by its electroforming that Fig. 2 is no ultra-thin metal layer.
Fig. 3 is the copper electroforming master tooling for having ultra-thin metal layer and the state diagram after the demoulding of the nickel part obtained by its electroforming.
Fig. 4 is demoulding state diagram when copper electroforming mold made from comparative example 1 is used for electroformed nickel part.
Fig. 5 is the surface scan figure of the ultra-thin metal layer of copper electroforming master tooling made from comparative example 2.
Specific embodiment
Now in conjunction with the drawings and specific embodiments, the present invention is further described.
Embodiment 1
A kind of preparation method of ultra-thin metal layer, includes the following steps:
Step 1 prepares electroforming solution: 100~150mmol/L KN03With 6~10mmol/L Pb (N03)2Matched using ultrapure water
System, electroforming solution temperature are controlled in (25 ± 1) DEG C.
Step 2, in advance press required shape made of the acetone soak oil removing of copper electroforming master tooling, then successively with anhydrous
Ethyl alcohol, ultrapure water are cleaned by ultrasonic 15~25 minutes；Be stereotype nitric acid dousing 10~15 seconds of 99.99% purity, then according to
Secondary progress ultrapure water is dried with nitrogen；
Copper electroforming master tooling is immersed in electroforming solution, cathode, anode by step 3 together as cathode, stereotype as anode
Between be powered, adjusting current density be 5~8.5A/dm2, carry out electro-deposition 0.5~2 second, make the surface shape of copper electroforming master tooling
At there is noncontinuity lead deposition layer (ultra-thin metal layer), transition region thickness is 0.2~1 μm, then takes out copper electroforming master tooling,
With the abundant rinsing, drying of deionized water, the ultra-thin metal layer preparation is completed；The copper electroforming master tooling is in use, ultra-thin gold
Belong to layer and is used as electroformed deposit face.
Technical effect in order to further illustrate 1 gained copper electroforming master tooling of embodiment has carried out comparative experiments: making respectively
With the copper electroforming master tooling of no ultra-thin metal layer, there is the copper electroforming master tooling (1 gained of embodiment) of ultra-thin metal layer to carry out nickel part
Then electroforming compares electroforming and completes front and back, the copper electroforming master tooling of no ultra-thin metal layer has the copper electroforming of ultra-thin metal layer female
Mould, the copper electroforming master tooling deposition gained nickel part through no ultra-thin metal layer, the copper electroforming master mold deposition institute for being had ultra-thin metal layer
State after the roughness of nickel part, demoulding, comparing result refer to Fig. 1-3, hence it is evident that as it can be seen that demoulding is very when not having ultra-thin metal layer
Arduously, and there is residual stress, be in rolled state after the demoulding of nickel part；When being prepared with ultra-thin metal layer (1 gained of embodiment), demoulding
Very laborsaving, residual stress substantially reduces, and is in straightened condition after the demoulding of nickel part.Therefore, 1 gained electroforming master tooling of embodiment both subtracted
The residual stress of few nickel part, and can be reduced roughness, and demould very laborsaving, hence it is evident that tearing is reduced, high-precision mould is suitable for
The electro-deposition of tool replicates.
Comparative example 1
The preparation method of the ultra-thin metal layer of comparative example 1 and embodiment 1 are almost the same, and difference is: preparing in comparative example 1
The concentration of electroforming solution is 20mmol/L.The electroforming of nickel part is carried out using the copper electroforming master tooling of comparative example 1, state when nickel part demoulds
Figure is as shown in Figure 4, it is seen then that due to the electroforming solution excessive concentration of comparative example 1, the metal ion in electroforming solution cannot achieve transient state at
Core carries out nickel using the copper electroforming master tooling of the state so that the ultra-thin metal layer formed on copper electroforming master tooling is overstocked blocked up
Part electroforming occurs being difficult to the phenomenon that demoulding, i.e., can not normal use, practicability is low, and the embodiment of the present invention 1 is completely absent
Aforementioned technical problem.
Comparative example 2
The preparation method of the ultra-thin metal layer of comparative example 2 and embodiment 1 are almost the same, and difference is: electric current in comparative example 2
Density is 15A/dm2.The electroforming of nickel part is carried out using the copper electroforming master tooling of comparative example 2, state diagram such as Fig. 5 when nickel part demoulds
It is shown, it is seen then that because although the current density of comparative example 2 can satisfy overpotential sedimentary condition, but due to current density mistake
Greatly, so that the ultra-thin metal layer that copper electroforming master tooling surface is formed forms sand-like graininess depositional phenomenon, electroforming is reduced instead
The precision on copper master tooling surface, is not available, and the embodiment of the present invention 1 is completely absent aforementioned technical problem.
Embodiment 2
A kind of preparation method of ultra-thin metal layer, includes the following steps:
Step 1 prepares electroforming solution: with 150~250mL secondary distilled water by 50~100g/L Zn0 and 150~300g/L
NaOH, which is stirred while hot to after dissolving completely, is diluted to 1~3L, and electroforming solution temperature is controlled in (25 ± 1) DEG C.
Step 2, in advance press required shape made of the acetone soak oil removing of copper electroforming master tooling, then successively with anhydrous
Ethyl alcohol, ultrapure water are cleaned by ultrasonic 15~25 minutes；Be zine plate nitric acid dousing 10~15 seconds of 99.99% purity, then according to
Secondary progress ultrapure water is dried with nitrogen；
Copper electroforming master tooling is immersed in electroforming solution, cathode, anode by step 3 together as cathode, zine plate as anode
Between be powered, adjusting current density be 10~15.5A/dm2, carry out electro-deposition 0.5~2 second, make the surface of copper electroforming master tooling
It is formed with noncontinuity zinc deposition layer (ultra-thin metal layer), transition region thickness is 0.2~1 μm, then takes out copper electroforming master mold
Tool, with the abundant rinsing, drying of deionized water, the ultra-thin metal layer preparation is completed；The copper electroforming master tooling is in use, ultra-thin
Metal layer is used as electroformed deposit face.
Electroforming master tooling made from the preparation method of the ultra-thin metal layer designed in summary, accuracy of repetition is excellent, replicates
Number is promoted, and the electro-deposition suitable for high-precision mold replicates, especially with the optical mould of micro-structure, preparation method letter
Single, preparation cost is low, is suitble to quantitatively promote the use of, practicability is high.
The foregoing descriptions are merely the embodiment using this origination techniques content, any those skilled in the art use this wound
Make done modifications and changes, all belong to the scope of the patents of this creation opinion, and is not limited to those disclosed embodiments.
Claims (13)
1. a kind of preparation method of ultra-thin metal layer, which comprises the steps of:
Step 1 prepares electroforming solution, and electroforming solution is the metal salt solution containing the metal ion for constituting ultra-thin metal layer；Electricity
Casting liquid is high concentration electroforming solution, its metal ion is gone back on matrix with transient state nucleation mode when high concentration electroforming solution is used for electroforming
It is former；
Step 2, the acetone soak oil removing of the matrix of depositing ultrathin metal layer is needed, then successively use dehydrated alcohol, ultrapure water
Ultrasonic cleaning 15-25 minutes；The metal plate for constituting ultra-thin metal layer with nitric acid dousing 10-15 seconds, then successively carry out
Ultrapure water is dried with nitrogen；
Matrix is immersed in electroforming solution by step 3 together as cathode, metal plate as anode, is powered between cathode, anode,
Current density adjusting is carried out, power supply can show that corresponding operating potential, control operating potential are higher than electroforming when current density is adjusted
The sedimentation equilibrium current potential of the metal ion of liquid, while operating potential is controlled lower than current potential is limited, limiting current potential is to guarantee electroforming solution
Metal ion not will form the current potential upper limit of sand-like particle deposition；It carries out electrodeposition time 0.5-40 seconds, on the surface of matrix
It is formed with ultra-thin metal layer, then takes out matrix, with the abundant rinsing, drying of deionized water, the ultra-thin metal layer preparation is completed.
2. the preparation method of ultra-thin metal layer according to claim 1, which is characterized in that step 1 middle and high concentration electroforming solution
Concentration using chronoamperometry determine: tested by electroforming solution of the chronoamperometry to various concentration, obtain it is each dense
The relation curve of the electric current i and response time t of the electroforming solution of degree, i.e. current versus time curve, according to the electroforming solution of each concentration
Current versus time curve obtains corresponding Limited diffusion current density im, time t used in the diffusion current density that reaches capacitym, with
Obtain the zero dimension of the electroforming solution of each concentrationRelation curve, by the zero dimension of the electroforming solution of each concentrationRelation curve and the zero dimension for judging nucleation modeTheoretical curve compares, when electroforming solution without because
It is secondaryThe zero dimension that relation curve becomes together in instantaneous nucleationWhen theoretical curve, the electricity of its corresponding concentration is judged
Cast liquid metal ion can transient state nucleation, that is, be determined to transient state nucleation high concentration electroforming solution concentration.
3. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: the metal of electroforming solution in step 3
Ion deposition equilibrium potential is determined using voltammetry, when electricity occurs in cathode current curve in the volt-ampere curve that voltammetry is presented
Flow ring when, corresponding to current potential, that is, electroforming solution metal deposit equilibrium potential.
4. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: limit current potential in step 3 and use
Current density continuously adjusts method and is determined, and power supply can show corresponding operating potential when current density is adjusted, then constantly continuous
Current density is improved, while observing the sedimentation state of the metal ion of electroforming solution, when there is sand-like particle deposition, corresponding work
Make current potential and limits current potential.
5. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: in step 3 to as cathode
Matrix carry out ultrasonic vibration, ultrasonic vibration frequency be 20-1000KHz.
6. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: in step 3 using pulse electricity
Stream, the duty ratio of pulse current are 20%-55%.
7. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: control carries out electricity in step 3
Sedimentation time is 0.5-2 seconds.
8. the preparation method of ultra-thin metal layer according to claim 7, it is characterised in that: described matrix is copper electroforming master mold
Tool；The copper electroforming master tooling is in use, ultra-thin metal layer is used as electroformed deposit face.
9. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: control carries out electricity in step 3
Sedimentation time is 10-40 seconds.
10. the preparation method of ultra-thin metal layer according to claim 9, it is characterised in that: described matrix is integrated circuit
Plate, the ultra-thin metal layer are used as conductive path.
11. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: the ultra-thin metal layer is lead
Layer, the concentration of electroforming solution are 6~10mmol/L, and current density is 5~8.5A/dm2。
12. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: the ultra-thin metal layer is zinc
Layer, the concentration of electroforming solution are 0.5~2mol/L, and current density is 10~15.5A/dm2。
13. the preparation method of ultra-thin metal layer according to claim 1, it is characterised in that: the thickness of the ultra-thin metal layer
Degree is less than 1 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811172751.6A CN109234769A (en) | 2018-10-09 | 2018-10-09 | A kind of preparation method of ultra-thin metal layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811172751.6A CN109234769A (en) | 2018-10-09 | 2018-10-09 | A kind of preparation method of ultra-thin metal layer |
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