CN106917116B - A kind of device and method of the sample preparation of metal foil high throughput and characterization - Google Patents
A kind of device and method of the sample preparation of metal foil high throughput and characterization Download PDFInfo
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- CN106917116B CN106917116B CN201710069647.3A CN201710069647A CN106917116B CN 106917116 B CN106917116 B CN 106917116B CN 201710069647 A CN201710069647 A CN 201710069647A CN 106917116 B CN106917116 B CN 106917116B
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
The present invention relates to metal foil preparation, characterization, systematic data accumulation and data intelligent applied technical field, in particular to a kind of device and methods of the sample preparation of metal foil high throughput and characterization.Described device includes the sample preparation of metal foil high throughput and characterizes complex control system, metal foil high throughput sample preparation system, metal foil high throughput sample characterization system, preparation and representation data-storage system and realize the connection system effectively connected between above-mentioned each system.Main feature and advantage of the present invention are, high-throughput thought and method are applied to the screening of metal foil production technology and optimization field, realize preparation, characterization and the data accumulation of automation, pipeline system metal foil high throughput sample, reducing human factor to greatest extent influences, shorten experimental period, efficiently completes the screening of metal foil production technology and Optimization Work.
Description
Technical field
The present invention relates to metal foil preparation, characterization, systematic data accumulation and data intelligent applied technical fields.It is special
It is not related to the device and method of a kind of sample preparation of metal foil high throughput and characterization.
Background technique
With the development of science and technology, demand of the fields such as electronic material, ornament materials to metal foil increasingly increases, electricity
Deposition generates metal foil in addition to keeping the performance of metal foil material of other methods production, when being prepared using electro-deposition method also
Can obtain according to demand by adjusting technique has the bright and clean, another side of one side more coarse (rough surface is convenient for pasting other materials
The surface of material increases binding force) or the bright and clean metal foil in two sides, surface shape controllability it is strong；Electro-deposition produces metal foil
Material can break through the limitation of rolling process production metal foil thickness, be easy to implement medium-scale production, be the life of energy conservation green relatively
At technique.Electrodeposit metals foil is widely used to the conductive material of printed wiring board, the electrolysis material of lithium battery, building dress
Exterior material, flexible bus, wave shield plate, high frequency busbar connector and thermal energy collect device etc..
The application demand different according to metal foil, needs the ingredient to metal foil, microstructure, thickness, table
Surface evenness (machine glazing, dual light etc.) etc. is many-sided to carry out fine adjustment, these adjustment are produced by metal foil
Plating solution composition (main salt, additive etc.), bath temperature, deposition current, anode and cathode spacing, bath flow rate in technique etc. it is a variety of because
Plain comprehensive regulation is realized.Based on the process control of known range it is still necessary to grope to attempt repeatedly, independent development new process
Orthogonal experiment screening and later period are huge to the performance characterization overall work amount of metal foil, take time and effort, cause new process development
Period is quite very long.Thus, there is an urgent need to develop the strong metal foil sample preparations of a kind of high efficiency, Modulatory character and characterization
Automatic assembly line formula experimental provision and method, to improve metal foil preparation process screening and optimization efficiency.
Summary of the invention
To solve the above problems, the present invention provides device and the side of a kind of sample preparation of metal foil high throughput and characterization
Method.Described device, can be efficient for realizing the automatic assembly line formula preparation of metal foil high throughput sample and performance characterization
Complete the screening of metal foil production technology and Optimization Work；High-throughput thought is applied to metal foil and produces work by the method
Skill screening and optimization, realize the Rapid Accumulation of the systematic data of technological parameter and its corresponding metal foil performance.
The present invention is achieved by the following technical solutions:
A kind of device of the sample preparation of metal foil high throughput and characterization, described device is for realizing metal foil high throughput
The automatic assembly line formula of sample prepares and performance characterization, efficiently to complete the screening of metal foil production technology and Optimization Work；
Described device includes:
Metal foil high throughput sample preparation system is continuously prepared from liquid phase banded with electrochemistry/chemical method
Metal foil high throughput sample, the technological parameter in the preparation process of the metal foil high throughput sample can automate continuously
Regulation；
Metal foil high throughput sample characterization system can carry out follow-on test table to the metal foil high throughput sample
Sign；
The sample preparation of metal foil high throughput and characterization complex control system, including metal foil high throughput sample preparation are comprehensive
Close control system and metal foil high throughput sample characterization complex control system；The metal foil high throughput sample preparation is comprehensive
Control system can as needed carry out the technological parameter in the metal foil high throughput sample preparation system automatic
Change continuous regulation；The metal foil high throughput sample characterization complex control system can be as needed to the high-throughput sample
Test and characterization equipment in characterization system send test instruction, and guarantee the metal foil prepared under different technical parameters
Material high throughput sample accurately passes through test and characterizes equipment and make the stop of right times, guarantees to metal foil high throughput sample
The accurate progress of performance characterization；
Connection system, for realizing data, the communication connection of instruction and the necessary object between system each in described device
Matter transmission.
Further, the metal foil high throughput sample preparation system includes metal foil sample preparation subsystem, work
Skill parameter regulates and controls subsystem and sample transfer, label and winding subsystem.
Further, the metal foil sample preparation subsystem includes electro-deposition cathode roll, cathode roll polishing and burnishing machine, arc
Shape anode plate, plating liquid pool, metal copper foil sample water lotion pond, metal copper foil sample cold wind sample drier.
Further, the technological parameter regulation subsystem includes bath composition/concentration measurement and control and comprehensive regulation component, electricity
Plate fluid flow pattern organization component in liquid pool, bath temperature regulatory component, current regulation component, the transmission of ribbon metal copper foil sample
Rate control component, anode and cathode distance regulation component；
The high throughput sample preparation and characterization complex control system pass through the regulation technological parameter and regulate and control subsystem pair
The technological parameter in the metal foil high throughput sample preparation system carries out automating continuous regulation.
Further, the sample transfer, label and winding subsystem include the transmission assembly of ribbon sample, positioning mark
Remember equipment and winding storage assembly.
Further, the metal foil high throughput sample characterization system includes metal foil high throughput properties of samples and property
Subsystem, sample transfer and winding subsystem can be characterized；
The metal foil high throughput properties of samples and performance characterization subsystem are to be integrated in metal foil height with modular
Throughput sample characterizes test and characterization equipment on system pipeline, the length of the assembly line, test wherein included and table
Levying equipment has scalability；Underlying table of the test with characterization equipment for metal foil is sought peace physical property measurement, Yi Jiqi
The combination of any one or any two kinds or more in the chemical/electrochemical performance detection in particular medium environment；
The sample transfer and winding subsystem and the metal foil high throughput sample preparation and characterization comprehensively control system
System connection, the metal foil high throughput sample preparation and characterization complex control system control under, the sample transfer with
Winding subsystem can control the traveling of metal foil high throughput sample and static, and guarantee is to metal foil high throughput properties of sample
The accurate progress of characterization.
Further, described device further include:
Preparation and representation data-storage system, including prepare data-storage system and characterize data storage system；The system
Standby data-storage system is used to store the technological parameter in the metal foil high throughput sample in each section of sample preparation procedure,
The characterize data storage system is used to store the characterize data of each section of sample in the metal foil high throughput sample.
Further, described device further include:
Intelligent data application system, retrieval of the intelligent data application system comprising data, calling, figure are aobvious
Show, data analysis, processing, excavate, it is customized screening, intelligence suggest at least one of functional software module；The intelligence
Data application system can be used alone, and customized metal foil manufacture process evaluation can be provided for researcher and is selected
The option of rule, and in the case where obtaining customized evaluation criterion, realize the intelligence of striping metal foil sample preparation technique
Energyization screening, provides process optimization suggestion.
High-throughput thought is applied to gold by a kind of method of the sample preparation of metal foil high throughput and characterization, the method
Belong to the screening of foil production technology and optimization, by metal foil high throughput sample preparation system to metal foil high throughput sample
Technological parameter in preparation process carries out automating continuous regulation, realizes the automatic assembly line formula of metal foil high throughput sample
Preparation, and pipeline system performance characterization is carried out to metal foil high throughput sample by high-throughput sample characterization system, realize work
The Rapid Accumulation of the systematic data of skill parameter and its corresponding metal foil performance；
The method can also be carried out wisdom data using area of computer aided and be sieved by intelligent data application system
Choosing, improves craft screening and efficiency is refined in optimization, data accumulation and rule.
Advantageous effects of the invention:
(1) high-throughput thought and method are applied to the screening of metal foil production technology and optimization field by the present invention, will
The screening of metal foil production technology and the sample preparation of optimization are converted into the continuous of ribbon sample with characterization conventional efficient problem
Preparation and representation, on the basis of existing metal foil manufacturing technique method, promoted the degree of automation, to processing parameter into
The control of row intelligent automation and adjusting, preparation includes the metal foil high throughput sample under the conditions of a large amount of different technical parameters,
Pass through the experimental provision and method, it is possible to reduce interference from human factor, it is high-throughput to complete metal foil for batch in the short time
The preparation of sample.
(2) performance test apparatus and device are openly integrated in modular form in characterization and test " assembly line ",
The selection of test equipment is flexible, scalability is strong, quickly and efficiently completes to be surface-treated ribbon metal foil in high-throughput sample
The characterization of product obtains metal foil performance data under the conditions of a large amount of different sample preparation technological parameters, fast implements in the short time
The Rapid Accumulation of the systematic data of technological parameter and its corresponding foil performance.
(3) wisdom data screening is carried out using area of computer aided, completes to high efficiency smart craft screening and optimization, data
Accumulation refines work with rule, greatly improves research and efficiency of research and development.
Detailed description of the invention
Fig. 1 is high-throughput sample preparation system schematic diagram in device of the present invention；
Fig. 2 is high-throughput sample characterization system schematic in device of the present invention；
Appended drawing reference: 1. plating liquid pools；2. bath temperature regulatory component；3. current regulation component；4. cathode roll polishing and burnishing machine；
5. plating solution tub；6. bath composition/concentration measurement and control and comprehensive regulation component；7. anode and cathode distance regulation component；8. cathode roll；9.
Arc-shaped anode plate；10. metal copper foil sample water lotion pond；11. fluid flow pattern organization component in liquid pool is electroplated；12. metal copper foil
Sample cold wind sample drier；13. the telltale mark equipment of ribbon metal copper foil sample；14. supporting and positioning wheel axis；15. electricity
Cable；16. ribbon metal copper foil sample transfer rate control assembly；17. central control computer；18. ribbon high throughput sample
Volume and bracket；19. metal surface pattern instrument；20. accurate hoistable platform bracket；21. conductivity metal measuring instrument；22.X ray is residual
Residue stress analyzer；23. full-automatic Vickers；24. wrap-up.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any substitution done on the essence and scope of the present invention being defined by the claims, repairs
Change, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to of the invention thin
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
The present invention can also be understood completely in description.
A kind of device of the sample preparation of metal foil high throughput and characterization, described device is by metal foil high throughput sample system
It is standby with characterization complex control system, metal foil high throughput sample preparation system, metal foil high throughput sample characterization system, system
It is standby to realize with characterize data storage system, intelligent data application system and between above-mentioned each system the connection system effectively connecting
System composition, it can be achieved that metal foil high throughput sample automatic assembly line formula preparation and performance characterization, and realize process data,
And the preparation of the high throughput tests pilot scale sample such as acquisition, storage, management, processing, analysis, excavation, recycling of performance characterization data, table
It seeks peace using whole process intelligent management.Efficiently, the screening of economic completion metal foil production technology and Optimization Work.
Include: in said device
(1) metal foil high throughput sample preparation system: mainly including metal foil sample preparation subsystem, technological parameter
Regulate and control subsystem, sample label and winding subsystem.Wherein:
The metal foil sample preparation subsystem includes electro-deposition cathode roll, the online rubbing down equipment of cathode roll, arc
Anode plate, plating liquid pool, washing liquid pool, cold wind sample drier etc., metal foil prepares subsystem with electrochemistry/chemical method
Ribbon metal foil high throughput sample is continuously prepared from liquid phase；
The technological parameter regulation subsystem includes in bath composition/concentration measurement and control and comprehensive regulation component, plating liquid pool
Fluid flow pattern organization component, bath temperature regulatory component, prepared using electrochemistry in the case of current regulation component, ribbon sample
Product transfer rate control assembly, anode and cathode distance regulation component etc., technological parameter regulate and control subsystem and metal foil sample preparation
Subsystem is attached by sensor or mechanical movement means, passes through sensor in metal foil high throughput sample preparation procedure
Monitoring carries out feedback control to technological parameter regulation subsystem, and subsequent technological parameter regulation subsystem is to the technique in preparation process
Parameter is controlled to adjust, and can carry out continuous control adjusting for a certain parameter, can also the coupling control and regulation of kinds of processes parameter；
The sample transfer, label and winding subsystem include the transmission assembly of ribbon sample, telltale mark equipment and
Storage assembly is wound, the transmission assembly of the ribbon sample may be implemented in metal foil high throughput sample preparation " assembly line "
Orderly transmission, the sample preparation of metal foil high throughput and controllable its transfer rate of characterization complex control system, pause duration
Deng；The telltale mark equipment is that ribbon metal foil high throughput sample is carried out positioning mark according to different technological parameters
Note characterize to the metal foil sample under various processes Parameter Conditions and then carries out metal foil production convenient for the later period
The screening and optimization of technique；The winding storage assembly completes the winding processing of sample after label, the storage group of arrangement winding here
Part is to make the two that can be distributed progress respectively, and can solve to increase the flexibility between high-throughput sample preparation and characterization connection
The problem of needing sample transmission speed, dead time that can not match there may be difference in sample preparation and performance characterization.I.e.
The characterization of metal foil high throughput sample does not carry out simultaneously with preparation, and ribbon metal foil high throughput sample is carried out winding storage
After depositing, then individually carry out metal foil high throughput sample characterization.
(2) metal foil high throughput sample characterization system: mainly including can be with above-mentioned high-throughput sample preparation system phase
High-throughput metal foil property match, modular and performance characterization subsystem group and sample transfer and winding subsystem.Its
In:
The test is with characterization equipment for surface physical properties test, material composition and crystal structure observation, vacuum item
It is tested under part and any one or any two or more combinations in particular solution in electrochemical behavior detection, for example survey
Examination with characterization equipment purposes include but is not limited to metal surface pattern, glossiness, roughness, surface profile, metallographic, hardness,
The performance test of the basic physics such as internal stress, conductivity and characterization, the observation of the spectroscopy such as Raman spectrum, infrared spectroscopy, X-ray diffraction
(XRD) etc. material compositions and crystal structure observation can even be swept after carrying out increasing vacuum conveyor system step by step to equipment
Retouch the vacuum conditions such as Electronic Speculum/power spectrum (SEM/EDS) observation, the observation of x-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES)
Under the electricity such as test and characterization, and open circuit potential (OCP), polarization curve, ac impedance spectroscopy (EIS) in particular solution
Chemical behavior test.The above test can be selectively integrated in characterization equipment according to specific performance testing requirement with modular
On " assembly line " of metal foil high throughput sample characterization system, wherein non-destructive testing or Non-destructive test equipment should be arranged in damage
Wound, before destructive testing equipment, the pipeline length and comprising test and characterization equipment there is extremely strong scalability,
It can add at any time as needed, for example, it is desired to can increase before metallographic microscope and invade when carrying out metallographic observation to sample surfaces
Liquid processing links (as realized using the methods of the etchant wiping of setting duration or spray) is lost, and adds washing, cold wind drying.?
Instruction of the equipment according to the sample preparation of aforementioned metal foil high throughput and characterization complex control system on " assembly line ", executes
Characterization task is directed across and does not execute characterization task, i.e., the equipment for only receiving test instruction executes test assignment.
The sample transfer and winding subsystem include a series of high-throughput metal foil samples supporting and positioning wheel axis and
Winding control component after test, it can be achieved that after the completion of " assembly line " test, for convenient for storage and to ribbon sample into
Row winding, while also supplement electro-deposition, supplement process or supplement test can be carried out to it with subsequent.
(3) preparation and representation data-storage system: the preparation and representation data-storage system is to store with characterize data
System data stores relevant module of software and hardware/equipment；In the sample preparation of metal foil high throughput and characterization complex control system
Coordinated control under, acquire the characterize data of sample preparation procedure process control parameter and all kinds of metal foil samples, together with when
Between, the information such as sample number into spectrum be stored in the storage hardware of host computer (or central control computer) together, guarantee data security, realize
Isomeric data fusion completes systematic data accumulation, in case subsequent calls, processing and analysis.
(4) intelligent data application system: intelligent data application system mainly includes to above-mentioned preparation and representation data
Data intelligent application in storage system, it may include but it is not limited to retrieval, calling, graphical display and the data analysis, place of data
The functional software modules such as reason, excavation, customized screening, intelligence suggestion, efficiently complete above-mentioned preparation and representation data-storage system
Middle data rule is refined, and provides researcher's option of customized metal foil manufacture process evaluation and selecting rule, and obtaining
In the case where defining evaluation criterion, realizes the intelligent screening of striping metal foil sample preparation technique, provide technique
Optimizing Suggestions.
(5) sample preparation of metal foil high throughput and characterization complex control system: as " brain " of whole device, in
Computer is controlled, and includes device comprehensively control software and man-machine dialog interface composition.Wherein the central control computer is responsible for entire
The time unification of device and the operation control for coordinating each systems/subsystems；Described device comprehensively control software is responsible for will be entire
Each system of device is got up by software contacts, so that the sample preparation of metal foil high throughput and characterization complex control system pass through dress
It sets comprehensively control software to operate electronic switch or mechanical device, and then realizes the coordinated control to whole device, simultaneously
Guarantee the correspondence between data and sample number into spectrum；The man-machine dialog interface realizes the " friendship of experimenter and whole device
Stream ".Experimenter carries out task program definition to experimentation using device comprehensively control software according to experimental design, coordinates fortune
The preparation and characterization experimental duties of ribbon metal foil high throughput sample are completed in row control.
(6) connect system: realize the connection system effectively connected between each system of the present invention mainly and include control cable,
Between the control and feedback interface of each system and subsystem, data transmission interface and data line and each system and subsystem
Interface communication protocol, water route connection, air circuit connection etc..The sample preparation of metal foil high throughput and table are realized by connection system
Levy complex control system to metal foil high throughput sample preparation system, metal foil high throughput sample characterization system, preparation with
Characterize data storage system, intelligent data application system are uniformly controlled；And by connection system, realize that metal foil is high
Gas circuit, water between throughput sample preparation system and each subsystem modules of metal foil high throughput sample characterization system
Docking, the extension of road, circuit, transmitted data line etc..
Coordinate operation mode in the present invention between each system is as described below:
The sample preparation of metal foil high throughput, which passes through with characterization complex control system as " brain " of whole device, to be connect
System realizes the coordinated control to system and subsystem, component each in whole device, and guarantees the time control of whole device, sample
Consistency in product number；Metal foil high throughput sample preparation system passes through various kinds of sensors and preparation and representation comprehensively control
System connection, utilizes the feedback of the monitoring data of various kinds of sensors and the experimental design of experimenter.
Experimental design of the experimenter based on system passes through the sample preparation of metal foil high throughput and characterization comprehensively control system
It unites and sequencing definition is carried out to the preparation and representation experiment of high-throughput sample, subsystem is regulated and controled by technological parameter and completes ribbon
Metal foil high throughput sample preparation, by control telltale mark system to the metal foil prepared under the conditions of different technical parameters
High-throughput sample carries out telltale mark, carries out winding storage to metal foil by winding system, in case carry out subsequent property and
Performance characterization, in preparation process generated all data, information recorded, uploaded by preparation and representation data-storage system,
It saves；Property when carrying out comprehensive characterization to foil high throughput sample, in metal foil high throughput sample characterization system " assembly line "
Matter and performance characterization equipment are connected with the sample preparation of metal foil high throughput with characterization complex control system, according to experimental arrangement
Design, selectivity call the detection on " assembly line " to execute test assignment according to specified process with characterization equipment, and " assembly line " stays
Expansion interface out can be extended as needed, and all data are by preparation and representation data caused by same sample characterization
Storage system record is uploaded, merges and is saved；Intelligent data application system is mainly in preparation and representation data-storage system
Data analyzed, excavated and provided intelligent suggestion.
A kind of method of the sample preparation of metal foil high throughput and characterization, the method are to combine high-throughput experiment theory will
The screening of metal foil production technology is converted into the continuous preparation and representation problem of ribbon sample with Optimization Work.The ribbon
The continuous preparation of sample is by adjusting to processing parameter intelligent automation stage, with electrochemistry/chemical method from liquid
Ribbon metal foil high throughput sample is continuously prepared in phase；The continuous characterization of the ribbon sample is will to test to set with characterization
Standby to be integrated on one " assembly line " with modular, the pipeline length, test wherein included have extremely strong with characterization equipment
Scalability, can add at any time as needed, utilize " assembly line " formula detection characterization equipment to ribbon metal foil high pass
It measures sample and carries out continuous detection characterization, sample is cut in change, then gradually carries out independent Experimental Characterization to the sample after cutting
Traditional experiment mode improves and realizes the matched flexibility of selectivity between each apparatus, improves sample characterization efficiency.It is logical
The control of Computerized intelligent precision is crossed, ribbon metal foil high throughput sample is passed sequentially through into the test on assembly line and is set with characterization
It is standby, efficiently complete the continuous characterization of ribbon sample, isomeric data is merged and is associated with and the works such as the storage of related system data
Make.The method also includes using intelligent data application system to related data carry out intelligent analysis processing, obtained from
In the case where defining evaluation criterion, process optimization suggestion and statistic analysis result are provided.
Embodiment 1
Fig. 1 is that metal foil high throughput sample preparation section shows in the device of the sample preparation of metal foil high throughput and characterization
It is intended to；A kind of specially electro-deposition specific embodiment for preparing metal copper foil high throughput sample, the preparation part includes metal
Copper foil high throughput sample preparation complex control system, metal copper foil high throughput sample preparation system, prepare data-storage system and
Connection system.It is described below:
1) metal copper foil high throughput sample preparation complex control system: main soft comprising central control computer 17 and its inside
Hardware module.Experimenter is intended to according to specific experiments, can carry out task program definition to experimentation by this system, realize
Time unification and coordinated operation to whole device, mainly to ribbon metal copper foil high throughput sample transfer rate, preparation/water
It washes/dries up technological parameter, Sample location label etc. to be adjusted, the preparation for completing ribbon metal copper foil high throughput sample is appointed
Business.
2) metal copper foil high throughput sample preparation system: regulate and control comprising metal copper foil sample preparation subsystem, technological parameter
Subsystem, sample transfer, label and winding subsystem.
(A) metal copper foil sample preparation subsystem: mainly including electro-deposition cathode roll 8, arc-shaped anode plate 9, electroplate liquid
Pond 1, metal copper foil sample water lotion pond 10, metal copper foil sample cold wind sample drier 12.
(a) cathode roll 8: the rotating metal roller as cathode when metal copper foil sample preparation, in direct current
Under the action of, just there is the absorption of metal copper ion to be formed on cathode roll and is electrolysed former foil, with the continuous rotation of cathode roll, generation
Former foil is continuously adsorbed and is removed on roller.
(b) arc-shaped anode plate 9: the arc seat board as anode when metal copper foil sample preparation, arcwall face is to cathode
Roller 8 has a fixed gap between arc-shaped anode plate 9 and cathode roll 8, centre, which is full of, crosses liquid.
(c) liquid pool 1: electrochemical reaction point when metal copper foil sample preparation is electroplated, is full of plating solution, and cathode roll 8, arc
Fluid flow pattern organization component 11, bath temperature regulatory component 2 etc. are mounted in plating liquid pool 1 in shape anode plate 9, plating liquid pool.
(d) metal copper foil sample water lotion pond 10: the metal copper foil of preparation is sprayed with deionized water, completely removes metal
Sample copper surfaces remain plating solution.
(e) metal copper foil sample cold wind sample drier 12: to the metal behind metal copper foil sample water lotion pond 10
Copper foil sample carries out cold air drying.
(B) technological parameter regulates and controls subsystem: in ribbon metal copper foil sample preparation procedure, metal copper foil high throughput sample
Preparation complex control system, which needs to regulate and control subsystem by technological parameter, carries out real-time monitoring to preparation technology parameter, to obtain
The high-throughput sample needed.It mainly includes following part that technological parameter, which regulates and controls subsystem: bath composition/concentration measurement and control and comprehensive regulation
Fluid flow pattern organization component 11, bath temperature regulatory component 2, current regulation component 3, ribbon metal in component 6, plating liquid pool
Copper foil sample transfer rate control assembly (also referred to as winding storage assembly) 16, anode and cathode distance regulation component 7, and cleaning with
Hot Air Dying Technology Parameters regulatory component etc..The technological parameter regulation subsystem is the core dress for preparing metal copper foil high throughput sample
It sets, is all implemented using computer program controlled automation, calculated by the middle control in metal copper foil preparation and representation complex control system
The conversion procedures of software human-computer interaction interface setting sample preparation technological parameter at any time, control technological parameter tune in machine 17
The movement of each component mechanical device or the folding of valve switch in subsystem are controlled, and then controls the change of technological parameter.Main packet
Containing following part:
(a) bath composition/concentration measurement and control and comprehensive regulation component 6: the bath composition/concentration measurement and control and comprehensive regulation group
Part 6 mainly controls concentration of metal ions, additive types and concentration etc. in plating solution.
(b) fluid flow pattern organization component 11 in liquid pool is electroplated: fluid flow pattern organization component 11 is main in the plating liquid pool
Flow of the electrolyte state and flow velocity in control plating liquid pool.
(c) bath temperature regulatory component 2: mainly the plating solution in liquid pool is electroplated in control to the bath temperature regulatory component 2
Temperature is stable at it within the scope of set temperature.
(d) current regulation component 3: the present embodiment needs in the case where preparing sample using electrochemical deposition method to anode and cathode
Between electric current regulated and controled, the current regulation component 3 mainly control current strength and current waveform.
(e) cathode roll polishing and burnishing machine 4: cathode roller surface aoxidizes in preparation process, for the metal foil material for guaranteeing preparation
Amount need to carry out rubbing down to cathode roll, and rubbing down is by the online rubbing down of cathode roll polishing and burnishing machine 4, metal foil produced during polishing
Equally carry out mark, record.
(f) ribbon metal copper foil sample transfer rate control assembly 16: the ribbon metal copper foil sample transmission speed
Mainly the revolving speed of control cathode roll revolving speed and matched wrap-up, realization are electric in the plating solution to sample for rate control assembly 16
The control of sedimentation time.
(g) anode and cathode distance regulation component 7: the anode and cathode distance regulation component mainly controls cathode roll and arc-shaped anode
The distance between plate, cathode roll enter liquid depth.
(h) sample clean and stoving process regulatory component: the sample clean mainly passes through with stoving process regulatory component
Metal copper foil sample water lotion pond 10 and metal copper foil sample cold wind sample drier 12 control scavenger in sample clean slot
Skill condition and subsequent cold air dryer stoving process condition, wherein cleaning process condition mainly includes water temperature, water (flow) direction and speed
Rate, water constituent etc.；Cold air dryer stoving process condition mainly includes flow constituents, drying wind size, temperature etc..
(C) sample transfer, label and winding subsystem: main includes the telltale mark equipment 13 and band of ribbon sample
Shape metal copper foil sample transfer rate control assembly (winding storage assembly) 16.
3) data-storage system is prepared: under being uniformly controlled of metal copper foil high throughput sample preparation complex control system,
The preparation technology parameter of every section of sample is uploaded to the data storage in specified host computer (being central control computer 17 in this example)
In database.
4) it connects system: realizing effective connection between each system, subsystem, mainly include control instruction and data transmission electricity
The control and feedback of each system of cable 15(and subsystem) and the corresponding interface and communications protocol, data transmission interface and data
Water route connection, air circuit connection in solution circulation, washing pool between line, plating solution tub 5 and plating liquid pool 1 in sprinkling equipment etc..
Ribbon metal copper foil high throughput sample preparation mainly includes following process flow:
S1 it) electro-deposition: is carried out in plating liquid pool 1, it should be noted that plating solution needs before entering plating liquid pool 1
Plating solution composition first is adjusted in plating solution tub 5, enter in electroplate liquid pond 1 after change plating solution composition in plating solution tub 5 and carry out
Electro-deposition.With the rotational speed of setting, anode plate 9 is kept at a distance from setting cathode roll 8 between cathode roll 8.
S2 when metal copper foil starts to continuously generate on cathode roll 8, cathode roll 8 and ribbon) removing and cleaning: are utilized
The pulling force that the rotation of metal copper foil sample transfer rate control assembly 16 generates, by being deposited on, the metal copper foil on cathode roll 8 is continuous
It strips down, remains plating solution on the metal copper foil stripped down, need to clean copper foil, finally in metal copper foil sample
It is sprayed in washing liquid pool 10 with deionized water, completely removes copper foil surface remnants plating solution.
S3) dry: behind metal copper foil sample water lotion pond 10, metal copper foil remained on surface has moisture, is unfavorable for it
Subsequent characterizations and storage need to dry it by metal copper foil sample cold wind sample drier 12 marking with before winding.
S4 it) marks: sample being marked using ribbon metal copper foil high throughput Sample location marking arrangement 13 after drying
Note.The telltale mark equipment 13 of the ribbon sample includes mainly a labelling machine, is placed on metal copper foil and prepares subsystem
It is high-throughput to the ribbon metal copper foil produced under the conditions of different technical parameters after metal copper foil sample cold wind sample drier
Sample carries out positioning one by one and labels with code printing, so as to record every section of sample the experiment date and technological parameter used, and it is rear
Enantiomorphic relationship one by one is established in the characterization of continuous metal foil high throughput sample and screening.
S5 it) winds: using supporting and positioning wheel axis 14 ribbon metal foil smoothly being slided, utilize ribbon metallic copper
Foil sample transfer rate control assembly 16 adjusts metal copper foil sample transfer rate, and to the copper foil high throughput sample after telltale mark
Product are wound, and are ready to carry out subsequent high pass amount sample characterization.
Fig. 2 is high-throughput sample characterization partial schematic diagram, band in the sample preparation of metal foil high throughput and characterization apparatus
Shape metal foil high throughput sample characterization mainly includes metal copper foil high throughput sample characterization complex control system, metal foil height
Throughput sample characterizes system, characterize data storage system and connection system.It is described below:
1) metal foil high throughput sample characterization complex control system: sending test instruction, and control metal foil is high-throughput
Performance characterization test of the sample on characterization " assembly line ", with the wrap-up control traveling of metal foil and static, guarantee is not
Metal foil sample with technological parameter preparation accurately passes through test in reasonable length and characterizes equipment and make right times
Stop, guarantee metal foil high throughput properties of sample measurement accurate progress, and with preparation technology parameter realize correspond.
2) metal foil high throughput sample characterization system: the core apparatus of metal foil high throughput sample characterization, it is main to wrap
Include metal foil high throughput properties of samples can match with high-throughput sample preparation, modular and performance characterization subsystem group
It (in the present embodiment include metal surface pattern instrument 19, accurate hoistable platform bracket 20, conductivity metal measuring instrument 21, X-ray
Analysis of Residual Stress instrument 22, full-automatic Vickers 23) and sample transfer and winding subsystem 24.Metal foil is high-throughput
Sample characterization system is matched with metal foil high throughput sample characterization complex control system, characterize data storage system, is realized
" assembly line " detection and acquisition, the storage of related data etc. to metal foil high throughput sample properties.
(A) metal foil high throughput properties of samples and performance characterization subsystem group: the high pass drawn from metal foil volume
Sampfe order is measured by metal foil high throughput properties of samples and performance characterization subsystem group, carries out characterization test.In this example
Metal foil high throughput properties of samples and performance characterization subsystem group include surface topography, conductivity, internal stress distribution, hardness four
Test is integrated on " assembly line " of metal foil high throughput sample characterization system with characterization equipment with modular by kind test,
The pipeline length, detection device wherein included have extremely strong scalability, can add at any time as needed, in " stream
The equipment also instruction according to the sample preparation of aforementioned metal foil high throughput and characterization complex control system on waterline ", executes table
Sign task is directed across and does not execute characterization task, i.e., the equipment for only receiving test instruction executes test assignment.
(B) sample transfer and winding subsystem: include ribbon metal foil high throughput sample volume and bracket 18, subsequent one
The supporting and positioning wheel axis 14 and the winding control component 24 after test of series of high-pass amount metal foil sample." assembly line "
After the completion of test characterization, mends and survey convenient for storage and subsequent high pass amount sample characterization.
3) it characterize data storage system: is controlled in the sample preparation of metal foil high throughput and the unified of characterization complex control system
Under system, the data that the various characterize datas of every section of sample are uploaded in specified host computer (being central control computer in this example) are deposited
It stores up in database, and corresponding with the realization of the preparation technology parameter of the sample.
4) it connects system: realizing effective connection between each system, subsystem, mainly include control instruction and data transmission electricity
The control and feedback of each system of cable 15(and subsystem) and the corresponding interface and communications protocol, data transmission interface and data line
Deng.
Specifically, metal foil high throughput sample characterization complex control system issues characterization test and data acquisition instructions
Afterwards, metal foil high throughput sample is tested as follows by each characterization equipment, sequence:
S1) surface topography is observed: surface topography observation is completed by metal surface pattern instrument 19, metal surface pattern instrument
It is connected with central control computer 17, measurement data Real time displaying stores and uploads central control computer.
S2) conductivity measurement: conductivity measurement is completed by conductivity metal measuring instrument 21, conductivity metal measuring instrument
21 included display screens are connected with central control computer 17, measurement data on-line storage, by conductivity metal measuring instrument 21 and accurate liter
It drops platform support 20 to be connected, accurate hoistable platform bracket 20 is connected with central control computer 17, and it is flat to control accurate lifting by computer
The lifting of platform bracket 20, and then the lifting that conductivity metal measuring instrument 21 is popped one's head in is controlled, complete metal foil high throughput sample
Conductivity characterizes, identical measure is also taken in data acquisition and upload, other instruments without autonomous lifting device, by instrument and precision
Hoistable platform bracket is connected.
S3) internal stress measuring: internal stress measuring is completed by automation X-ray analysis of Residual Stress instrument 22, automates X
Ray residual stress analysis instrument 22 can fast and accurate measurement metal foil high throughput sample internal stress distribution, within measurement form
Stress distribution expression, automation X-ray analysis of Residual Stress instrument 22 are connected with central control computer 17, are controlled by computer computer
The work of system automation X-ray analysis of Residual Stress instrument 22, internal stress characterization, the data for completing metal foil high throughput sample are adopted
Collection and upload.
S4) hardness measurement: hardness measurement is carried out by full-automatic Vickers 23, full-automatic Vickers 23 with
Central control computer 17 is connected, and by metal foil high throughput sample by full-automatic Vickers 23, is controlled by central control computer 17
Controlling rolling device 24 stop and the residence time, with this come complete metal foil high throughput sample hardness characterization, data acquisition with
It uploads.
S5) wind: the middle control that wrap-up 24 is controlled by metal foil high throughput sample characterization complex control system calculates
Machine 17, the movement of regulation wrap-up and stopping.
Can there are the metal foil prepared under the conditions of two kinds of process conditions superpositions, this section of metal when switching production technology
Foil can be studied not, but as function admirable can also be included in research vision.
By in above-mentioned Fig. 1 and metal foil high throughput sample preparation shown in Fig. 2 and characterization apparatus preparation part and table
Sign part combines；For a complete example of ribbon metal foil high throughput sample electro-deposition preparation and representation in the present invention.
Claims (9)
1. a kind of device of the sample preparation of metal foil high throughput and characterization, which is characterized in that described device is for realizing metal
The automatic assembly line formula of foil high throughput sample prepares and performance characterization, with efficiently complete the screening of metal foil production technology with
Optimization Work；
Described device includes:
Metal foil high throughput sample preparation system continuously prepares banded metal with electrochemistry/chemical method from liquid phase
Foil high throughput sample, the technological parameter in the preparation process of the metal foil high throughput sample can automate continuous tune
Control carries out positioning one by one to the ribbon metal copper foil high throughput sample produced under the conditions of different technical parameters and pastes with code printing
Mark, so as to record every section of sample the experiment date and technological parameter used, with the characterization of subsequent metal foil high throughput sample with
Enantiomorphic relationship one by one is established in screening；
Metal foil high throughput sample characterization system, test are integrated in metal foil high throughput sample with characterization equipment with modular
On the assembly line of characterization system, pipeline system follow-on test characterization can be carried out to the metal foil high throughput sample；
The sample preparation of metal foil high throughput and characterization complex control system, including the comprehensive control of metal foil high throughput sample preparation
System processed and metal foil high throughput sample characterization complex control system；The metal foil high throughput sample preparation comprehensively control
System can carry out automation company to the technological parameter in the metal foil high throughput sample preparation system as needed
Continuous regulation；The metal foil high throughput sample characterization complex control system can be as needed to the high-throughput sample characterization
Test and characterization equipment in system send test instruction, and guarantee the metal foil prepared under different technical parameters height
Throughput sample accurately passes through test and characterizes equipment and make the stop of right times, guarantees to metal foil high throughput properties of sample
The accurate progress of characterization；
Connection system passes for realizing data, the communication connection of instruction and the necessary substance between system each in described device
It send.
2. a kind of device of the sample preparation of metal foil high throughput and characterization according to claim 1, which is characterized in that described
Metal foil high throughput sample preparation system includes metal foil sample preparation subsystem, technological parameter regulation subsystem and sample
Transmission, label and winding subsystem.
3. a kind of device of the sample preparation of metal foil high throughput and characterization according to claim 2, which is characterized in that described
Metal foil sample preparation subsystem includes electro-deposition cathode roll, cathode roll polishing and burnishing machine, arc-shaped anode plate, plating liquid pool, gold
Belong to copper foil sample and washes liquid pool, metal copper foil sample cold wind sample drier.
4. a kind of device of the sample preparation of metal foil high throughput and characterization according to claim 2, which is characterized in that described
Technological parameter regulation subsystem includes fluid flow pattern tissue in bath composition/concentration measurement and control and comprehensive regulation component, plating liquid pool
Component, bath temperature regulatory component, current regulation component, ribbon metal copper foil sample transfer rate control assembly, anode and cathode
Distance regulation component；
The high throughput sample preparation regulates and controls subsystem to described by regulating and controlling the technological parameter with characterization complex control system
The technological parameter in metal foil high throughput sample preparation system carries out automating continuous regulation.
5. a kind of device of the sample preparation of metal foil high throughput and characterization according to claim 2, which is characterized in that described
Sample transfer, label and winding subsystem include the transmission assembly of ribbon sample, telltale mark equipment and winding storage group
Part.
6. a kind of device of the sample preparation of metal foil high throughput and characterization according to claim 1, which is characterized in that described
Metal foil high throughput sample characterization system includes metal foil high throughput properties of samples and performance characterization subsystem, sample transfer
With winding subsystem；
The metal foil high throughput properties of samples and performance characterization subsystem are that metal foil high throughput is integrated in modular
Test on sample characterization system pipeline and characterization equipment, the survey for including in the length of the assembly line and the assembly line
Examination has scalability with characterization equipment；Underlying table of the test with characterization equipment for metal foil is sought peace physical property measurement, with
And its combination of any one or any two kinds or more in the chemical/electrochemical performance detection in particular medium environment；
The sample transfer and winding subsystem and the metal foil high throughput sample preparation and characterization complex control system connect
It connects, under the metal foil high throughput sample preparation and the control of characterization complex control system, the sample transfer and winding
Subsystem can control the traveling of metal foil high throughput sample with it is static, guarantee to characterize metal foil high throughput properties of sample
Accurate progress.
7. any one of -6 a kind of device of the sample preparation of metal foil high throughput and characterization according to claim 1, feature
It is, described device further include:
Preparation and representation data-storage system, including prepare data-storage system and characterize data storage system；It is described to prepare number
It is used to store the technological parameter in the metal foil high throughput sample in each section of sample preparation procedure according to storage system, it is described
Characterize data storage system is used to store the characterize data of each section of sample in the metal foil high throughput sample；Same section of sample
The preparation data of product are corresponded to each other with characterize data, convenient for intelligent data application system mining data rule, instruct technique excellent
Change.
8. any one of -6 a kind of device of the sample preparation of metal foil high throughput and characterization according to claim 1, feature
It is, described device further include:
Intelligent data application system, the intelligent data application system include the retrieval of data, calling, graphical display, number
According to the functional software module of at least one of analysis, processing, excavation, customized screening, intelligence suggestion；The intelligent data is answered
It with system, can be used alone, customized metal foil manufacture process evaluation and selecting rule can be provided for researcher
Option, and in the case where obtaining customized evaluation criterion, realize the intelligent sieve of striping metal foil sample preparation technique
Choosing, provides process optimization suggestion.
9. a kind of method of the sample preparation of metal foil high throughput and characterization, the method is using any one of claim 1-8 institute
State device, which is characterized in that high-throughput thought is applied to the screening of metal foil production technology and optimized by the method, is passed through
Metal foil high throughput sample preparation system carries out the technological parameter in the preparation process of metal foil high throughput sample automatic
Change continuous regulation, realize the automatic assembly line formula preparation of metal foil high throughput sample, and passes through high-throughput sample characterization system
System carries out pipeline system performance characterization to metal foil high throughput sample, realizes technological parameter and its corresponding metal foil performance
Systematic data Rapid Accumulation；
The method can also be carried out wisdom data screening using area of computer aided, be mentioned by intelligent data application system
High technology screening refines efficiency with optimization, data accumulation and rule.
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| CN108362849A (en) * | 2017-12-19 | 2018-08-03 | 成都亦道科技合伙企业（有限合伙） | A kind of high-throughput screening method of alloy collector |
| CN109827940B (en) * | 2018-12-21 | 2021-03-16 | 中山大学 | In-situ characterization method and device for light-electric excitation electron emission |
| CN109811373B (en) * | 2019-02-25 | 2021-01-15 | 赣州逸豪新材料股份有限公司 | Electrolytic copper foil raw copper foil machine with cathode roller synchronous finishing function |
| CN111172566B (en) * | 2020-02-17 | 2020-11-03 | 广东嘉元科技股份有限公司 | Production process for eliminating white spots of electrolytic copper foil, foil forming machine and pole distance control method |
| CN113909044B (en) * | 2021-09-18 | 2022-11-08 | 惠州中京电子科技有限公司 | High-flux preparation system and method for PCB substrate |
| CN113984481B (en) * | 2021-11-11 | 2024-01-23 | 中国核动力研究设计院 | Device and method for preparing performance characterization sample |
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