CN101342525A - Method for preparing combined material chip and electromagnetic injection system used - Google Patents
Method for preparing combined material chip and electromagnetic injection system used Download PDFInfo
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- CN101342525A CN101342525A CNA2008100423227A CN200810042322A CN101342525A CN 101342525 A CN101342525 A CN 101342525A CN A2008100423227 A CNA2008100423227 A CN A2008100423227A CN 200810042322 A CN200810042322 A CN 200810042322A CN 101342525 A CN101342525 A CN 101342525A
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Abstract
本发明涉及一种制备组合材料芯片的方法及所使用的系统，其特征在于可溶物溶液或难溶物悬浮液预先在溶液管路中混合均匀，然后用外界气体驱动的电磁式喷射系统，将混合均匀的可溶物溶液或难溶物悬浮液喷射到基板上，通过热处理制备成组合材料芯片。所使用的电磁喷射系统由管路系统和定位系统构成。在电磁泵的驱动下充分混合后于混合池中获得不同组成的样品，由电磁喷头喷出；电磁喷头固定于喷头升降架上，喷头相对于基板的高度由喷头升降架调节；基板固定于二维X－Y电动平台上，二维电动平台水平放置，喷头升降架和二维电动平台固定在同一工作平台，单片机通过电动平台的控制器驱动二维电动平台，通过电磁阀的控制驱动器控制电磁阀的开闭。
The invention relates to a method for preparing composite material chips and the system used, which is characterized in that the solution of soluble matter or the suspension of insoluble matter is uniformly mixed in the solution pipeline in advance, and then an electromagnetic spraying system driven by external gas is used, Spray the uniformly mixed soluble solution or poorly soluble suspension onto the substrate, and prepare a combined material chip by heat treatment. The electromagnetic injection system used consists of a piping system and a positioning system. After being fully mixed under the drive of the electromagnetic pump, samples of different compositions are obtained in the mixing tank, which are sprayed out by the electromagnetic nozzle; the electromagnetic nozzle is fixed on the nozzle lifting frame, and the height of the nozzle relative to the substrate is adjusted by the nozzle lifting frame; the substrate is fixed on the two On the dimensional X-Y electric platform, the two-dimensional electric platform is placed horizontally, the nozzle lifting frame and the two-dimensional electric platform are fixed on the same working platform, the single-chip microcomputer drives the two-dimensional electric platform through the controller of the electric platform, and the solenoid valve is controlled by the control driver. valve opening and closing.
Description
Technical field
The present invention relates to prepare the method and the employed electromagnetic spray system of combined material chip, mainly be by spraying preceding method, preparing the parallel synthesizer and the using method in material sample storehouse when belonging to the combined sorting new material with DDGS solution or mixing of indissoluble thing suspension and injection.
Background technology
Combined method is a kind of method of efficient screening new material.Adopt combined method, can on a substrate, synthesize the material sample of a large amount of different components simultaneously, constitute a huge and intensive material sample array, i.e. material chip (claiming the material sample storehouse again).This method of synthetic lot of materials sample simultaneously is called parallel synthetic.
Existing parallel synthetic method mainly can be divided into Film forming method and liquid phase method two big classes.Wherein liquid phase method mainly is by moving the liquid technology different solution to be injected different microreactors in the ratio of setting, synthetic different materials.Relatively more successful is droplet discharge technique at present.
And droplet discharge technique is divided into piezoelectric type and drives injection, and thermal bubble type drives injection and the electromagnetic type driving is sprayed.Thereby piezoelectric type is sprayed and is adopted ceramic polycrystalline piezoelectric patches at shower nozzle generation pressure liquid to be sprayed.Thermal bubble type sprays and is meant that the pressure that produces after the bubble that utilizes the transient liquid boiling to generate by heating liquid breaks sprays liquid.These two kinds of technology are used for the parallel synthetic of material chip, are to obtain different materials by different liquid is sprayed into to mix in the different microreactors according to the ratio of setting again by post processing.Reported indissoluble thing suspension injection method and the device that is used to prepare the combined material sample library as Chinese patent CN1603011 and CN2759615, the pressure-driven liquid that promptly adopts piezoelectric ceramics to produce sprays from shower nozzle, the solution spraying system that utilizes piezoelectric type or thermal bubble type technical scheme to make is easy to operate simple, but for the bigger indissoluble thing suspension of viscosity, the driving force deficiency that one side piezoelectric type or thermal bubble type produce, the amount that is difficult to effectively ejection or ejection has certain randomness to be difficult to accurate control; On the other hand, what this dual mode adopted is to spray the back to mix, so the bigger indissoluble thing suspension of viscosity is difficult for mixing in microreactor and is easy to generate component segregation.Contrast above two kinds of technical schemes, it then is to provide driving force such as gas pressure to reach the purpose of mixing and injection by the switching of solenoid control feed flow pipeline and control shower nozzle by outer bound pair liquid that electromagnetic type is sprayed.The amount that the amount of liquid of different component and shower nozzle spray can be by the liquid driven power control different with adjusting of different switching time of magnetic valve.Ejection again after the liquid injection system of Electromagnetic Drive can mix different liquid on principle before injection, the different proportion that different liquid is set can realize by the different switching time of control magnetic valve, and such pattern not only can guarantee the abundant mixing of solution or indissoluble thing suspension but also can reach the purpose of injection by regulating driving force.This just is guided out purpose of the present invention.
Summary of the invention
The object of the present invention is to provide a kind of method and electromagnetic spray system for preparing combined material chip.
The solution spraying technique of utilizing that the present invention is different from is in the past carried out the method for material chip preparation, and maximum improvement is to mix the pattern of spraying then with spraying before the pattern of mixing in the microreactor back becomes injection in the solution pipeline on substrate.Spray the pattern that mix the back, usually need to adopt to stir, ultrasonic, means such as rock and promote the mixing of liquid in microreactor, apparent, for the solution of good fluidity, these means can promote to mix preferably, but for the indissoluble thing suspension of thickness comparatively and mobile difference, these methods just can not make liquid mix fully, and are easy to generate component segregation after the heat treatment.Therefore be that the indissoluble thing suspension that mixes the mobile difference of thickness is fully mixed in the pipeline that designs, thereby fundamentally overcome the problem of the component segregation that when mixing, easily produces after the injection.Another improvement of the present invention is the shower nozzle drive pattern of piezoelectric type is changed into the drive pattern of air pressure electromagnetic type.The spraying system advantage of Piezoelectric Driving pattern is simple in structure, easy to maintenance, but for the bigger indissoluble thing suspension of viscosity, the driving force deficiency that the one side piezoelectric type produces, be difficult to effective ejection, Pen Chu amount has certain randomness to be difficult to accurate control simultaneously; On the other hand, increasing Piezoelectric Driving power needs higher voltage, will certainly improve user's security risk like this, simultaneously, the driving force of piezo jets is fixing when making, and can not regulate flexibly at different liquid, will certainly limit its performance like this.By comparison, the air pressure electromagnetic type is that a kind of driving force such as gas pressure that utilizes outer bound pair liquid to provide reaches the purpose of mixing and spraying by solenoid control feed flow pipeline and the switching of controlling shower nozzle.The amount that the amount of liquid of different component and shower nozzle spray can be by the liquid driven power control different with adjusting of different switching time of magnetic valve.The power resources of the electromagnetic type liquid injection system that air pressure drives on principle are in ambient atmos pressure, can carry out pressure so safely and easily regulates, the feasible driving force that can select easily to mate at different liquid is sprayed, ejection again after different liquid can being mixed before injection simultaneously, the different proportion that different liquid is set can be realized by the different switching time of control magnetic valve, this point is different from liquid injection system in the past as mentioned above, so the pattern of air pressure electromagnetic type not only can guarantee the abundant mixing of solution or indissoluble thing suspension but also can reach the purpose that control is sprayed by regulating driving force.It is that structure and maintenance are comparatively complicated that obvious such selection also has certain shortcoming.
DDGS solution of the present invention is all DDGS solution, and DDGS is at the simple substance of specific solvent or compound.
Indissoluble thing of the present invention comprises as oxide, sulfide, carbide, nitride, chloride, fluoride, carbonate, sulfate, silicate etc. (as TiO
2, Nb
2O
5, Bi
2O
3, ZnS, SiC, BC, SiN, BN, AgCl, CaF
2, BaF
2, BaCO
3, CaCO
3, BaSO
4, CaSiO
3).
In sum, the present invention is intended to provide a kind of liquid jet method for preparing combined material chip, and to propose a kind of DDGS solution for preparing the combined material sample library or indissoluble thing suspension spraying system according to the method be that the liquid phase method of raw material is parallel synthetic to realize with DDGS solution or indissoluble thing.
Essence of the present invention is that the technology of preparing with droplet discharge technique and indissoluble thing suspension combines, and is used for from indissoluble raw material making material chip.Integrated by both, needed solution or the vectored injection of indissoluble composition granule can be arrived the appropriate location of material base, thereby realize the material chip printing.
Core concept of the present invention is to spray the uneven problem of mixing that the back hybrid plan exists by the first method that the suspension of DDGS solution or indissoluble thing is mixed before injection in the prior art to overcome, its maximum characteristics are that system is an open platform, by increasing the unit number of liquid-supplying system, can realize that binary arrives the parallel synthetic of multicomponent mixture, promptly the user can improve system according to own needs; Air pressure electromagnetic type drive pattern system with more control parameter also provides an extendible platform for the user.
For this reason, the present invention also provides and has realized the above-mentioned employed electromagnetic spray system of method for preparing combined chip.
Electromagnetic spray system provided by the present invention is made up of pipe-line system and navigation system.
Wherein, described pipe-line system comprises that gas piping, liquid line, flow-control magnetic valve and hybrid electromagnetic pump constitute the injection navigation system and then be made up of the controller of two-dimentional X-Y electric platforms and electric platforms.
Described gas piping is made up of sample air inlet pipe, injection air inlet pipe and cleaning fluid air inlet pipe, desire mixing DDGS solution or indissoluble thing solution are placed on liquid storage tank according to need respectively and are connected, spray air inlet pipe and link to each other with mixing pit, the cleaning fluid air inlet pipe is connected with the cleaning liquid pool; The pressure that uses ambient atmos to inject, mix and spray as liquid; Use magnetic valve to carry out the control of fluid flow, the liquid that uses the electromagnetic type shower nozzle to carry out mixed DDGS solution or indissoluble thing solution sprays, and the mixing of liquid is implemented by electromagnetic pump.
Realize the preparation of binary or multicomponent material chip by the quantity of increase and decrease air inlet pipe, liquid storage tank and feed tube.
Liquid line is made up of the connecting pipe that connects liquid storage tank, sample feed tube, mixing pit, electromagnetic pump and mixing pit, cleaning liquid pool, wherein liquid storage tank is connected with mixing pit by the sample feed tube, electromagnetic pump is connected with mixing pit by connecting pipe, cleans liquid pool and is connected with mixing pit.The flow-control magnetic valve is by the sample magnetic valve that is connected with the sample feed tube, the cleaning fluid magnetic valve that is connected with the cleaning fluid feed tube, with the electromagnetic pump that mixing pit is connected by connecting pipe, with the three-way magnetic valve that the injection air inlet pipe is connected, the electromagnetism shower nozzle that is connected with mixing pit is formed.Under external gas pressure drives, solution or indissoluble thing suspension that Pneumatic pipe cleaner is crossed DDGS in the air inlet pipe promotion liquid storage tank enter mixing pit by feed tube, the amount of utilizing the open and close controlling of the magnetic valve that feed tube connects to enter the different solutions or the suspension of mixing pit, mixing pit is by mixing chamber, mixing striker and pipe joint forms, mixing chamber is cylindrical, mix striker and be positioned at the pipe joint liquid outlet, pipe joint connects feed tube, air inlet pipe, electromagnetic pump and mixing pit connecting pipe and electromagnetism shower nozzle, mix by electromagnetic pump and with the DDGS solution or the indissoluble thing suspension of mixing pit connecting pipe, provide gas pressure to promote DDGS solution or the ejection of indissoluble thing suspension process electromagnetism shower nozzle in the mixing pit by air inlet pipe through three-way magnetic valve to mixing pit; Promote to clean by air inlet pipe that cleaning fluid enters mixing pit in the liquid pool, start electromagnetic pump clean electromagnetic pump and with the mixing pit connecting pipe, clean waste liquid and under three-way magnetic valve provides gas pressure, spray by the electromagnetism shower nozzle, clean the electromagnetism shower nozzle simultaneously.The electromagnetism shower nozzle is fixed on the shower nozzle crane, and the electromagnetism shower nozzle is regulated by the shower nozzle crane with respect to the height of substrate.
Described mixing pit, mixing striker are made by polytetrafluoroethylmaterial material.
Described injection navigation system is made up of two-dimentional X-Y electric platforms and electric platforms control system.Wherein mixing pit and electromagnetism shower nozzle are fixed on the two-dimentional X-Y electric platforms by the shower nozzle crane, and substrate is fixed on the two-dimentional X-Y electric platforms, two-dimentional X-Y electric platforms horizontal positioned, and shower nozzle crane and two-dimentional electric platforms are fixed on the same workbench.Drive by the electric platforms controller by single-chip microcomputer.
The electric platforms control system is made up of single-chip microcomputer, electric platforms controller, control driver element and interlock circuit etc.
Wherein, control single chip computer drives two-dimentional electric platforms, controls the switching that drives magnetic valve, three-way magnetic valve, electromagnetic pump, electromagnetism shower nozzle by the control driver element of magnetic valve, three-way magnetic valve, electromagnetic pump, electromagnetism shower nozzle by the electric platforms controller.
Circuit part mainly by: single chip circuit, liquid crystal display circuit, keyboard circuit, driving circuit for electromagnetic valve, stepper motor driving circuit and power circuit six parts are formed.By LCD interface control LCD, by the action of the moving device interface control step motor of stepper motor, by driving circuit for electromagnetic valve control and the work of driving magnetic valve.The circuit theory of electromagnetic spray system is referring to shown in the accompanying drawing 3.
Adopt the PIC16C77 single-chip microcomputer, the clock circuit of SCM system adopts passive crystal oscillator to connect two electric capacity, and the oscillating circuit in conjunction with single-chip microcomputer inside constitutes complete oscillating circuit again, as shown in Figure 4.As system clock source, so the clock cycle of system is 0.25 μ s, an instruction cycle was made up of 4 clock cycle, i.e. 1 μ s with the quartz crystal oscillator of 4MHz.Except designed a system clock circuit for spraying system, also for counter Timer1 has designed an outer clock circuit, also be to adopt passive crystal oscillator to connect two electric capacity, the oscillating circuit in conjunction with single-chip microcomputer inside constitutes complete oscillating circuit again.As the clock source, the 1s clock that is used to the standard that produces interrupts, and controls the switch time of LCD backlight with the quartz crystal oscillator of 32.768KHz.Single chip circuit and pin function are referring to accompanying drawing 4.
The main effect of liquid crystal display circuit is: the parameter that shows combined jet equipment is provided with situation and shows current working state.LCD adopts is the Xiamen height GDM0801A-FL-YBS LCD that Optical Co., Ltd produces of standing upright, and single file shows 8 characters, and each character is 5 * 8 dot matrix and has blinking cursor.Be in the control core circuit with the PIC single-chip microcomputer, this backlight liquid crystal display lamp is the components and parts of consumed power maximum.When backlight is in opening for a long time, very serious heating phenomenon can appear in 7805 voltage-stabiliser tubes in the power circuit, serious in order to prevent the heating of 7805 voltage-stabiliser tubes, simultaneously also in order to reduce the power consumption of spraying system, designed the circuit of closing backlight automatically for LCD specially, FET IRF640 among the figure is used for controlling the LCD backlight lamp specially and opens and closes, it is equivalent to a switch that is between backlight negative pole and the ground, controls the break-make of IRF640 by the RA2 mouth of PIC single-chip microcomputer.Realize by the liquid crystal control program: when in 30s, do not press keyboard, the LCD backlight lamp will be closed automatically.FET IRF640 is the N channel-type, maximum withstand voltage 200V between drain-source, conducting resistance 180 Ω, drain electrode maximum current 18A.LCD pin function and peripheral circuit are referring to accompanying drawing 5.
Keyboard circuit is mainly used in the setting of combined jet synthesis device parameter and the duty of control printer.The keyboard pin function is seen shown in the accompanying drawing 6.One has 5 buttons, is respectively the procedure Selection key, increases progressively key, the key that successively decreases, determines key (hold concurrently and be the cursor shift key) and reset key.Options button is used for the selection of function menu; The key that successively decreases is used to increase parameter value; The key that successively decreases is used to reduce parameter value; Determine that key is used to control the duty of printer, for example make printer begin to spray, suspend and spray and stop to spray, determine key double as cursor movement key simultaneously, when carrying out using its moving cursor when parameter is set; Reset key is used to restart single-chip microcomputer, receives when printer and disturbs and can press reset key when causing work undesired and make printer return to original state, restarts to spray.
The product of the U.S. Lee company that magnetic valve, electromagnetism shower nozzle and electromagnetic pump adopt, its rated operational voltage is 12V or 24V, the present invention is its design driven circuit, to guarantee the operate as normal of magnetic valve.Driving circuit for electromagnetic valve as shown in Figure 7.Component shown in the figure is all the universal electric element, and model as shown in the figure.The input signal of driving circuit for electromagnetic valve is sent by the PIC single-chip microcomputer, and output signal has two power supply V1 and V2, is called respectively to keep voltage and impulse voltage.Impulse voltage is used to activate magnetic valve, keeps voltage to be used for maintaining valve and is in opening for a long time.This drive circuit both can be used as enhancing response drive circuit and also can be used as the low-power consumption drive circuit.V1 is the rated operational voltage (24V) of magnetic valve when as enhancing response drive circuit, and the value of V2 is 2～4 times of rated operational voltage.The response speed of the big more magnetic valve of the value of V2 is also just fast more.When as low consumption circuit, the V1 value is half of rated operational voltage, and V2 is the rated operational voltage of magnetic valve.Power consumption can be reduced by 75% like this, what spraying system provided by the invention adopted is this low-power consumption mode.The input and output waveform of drive circuit as shown in Figure 8.This drive circuit is realized the modulation of signal output waveform through the capacitor C 300 at signal input port place and triode Q300 and NE555 timer, and NE555 adopts pulse enable monostable, total service time t
1By the control signal decision of single-chip microcomputer, can control t flexibly by software programming
1Size.Impulse time t
2With retention time t
3Adjustment realize t by NE555 timer hardware
2=1.1 * R
302* C
302, by adjusting R
302And C
302Value, just can adjust t
2And t
3Size.Generally be capacitor C
302Be fixed as 1uF, by adjusting potentiometer R
302The waveform that obtains to want.
The driver of stepper motor is to be manufactured and designed by Shanghai laser research institute, links to each other with the PIC single-chip computer control system by signal cable line DB25.PIC controls the move left and right of X-Y platform and the speed that moves to the driver sending controling instruction.
Power unit is the most basic circuit part of entire circuit system, is responsible for whole system stable voltage is provided, and the quality of its design is directly connected to the reliability and the stable state of whole spraying system.In order to guarantee the stable of supply voltage; power module adopts the circuit of three-terminal voltage-stabilizing integrated of 78 series; it is few to form the required peripheral cell of voltage-stabilized power supply with 78 serial three-terminal voltage-stabilizing IC, and circuit is inner to also have overcurrent, overheated and adjust the holding circuit of pipe, uses reliable, convenient.Whole system needs three power supplies altogether, as shown in Figure 9.
It is as follows that each organizes the effect of power supply:
1.+5V power supply: be power supplies such as PIC16C77 single-chip microcomputer and peripheral module such as latch 74LS374, electromagnetism shower nozzle, three-way solenoid valve;
2.+12V power supply: be timer NE555 power supply, be used as the working power of magnetic valve simultaneously;
3.+24V power supply: be the electromagnetic pump power supply, be used as the activating power of magnetic valve and electromagnetism shower nozzle simultaneously.
The invention using method:
After required solution or suspension mixed in hybrid chamber according to different proportionings, at the desired location metered injection, the preparation material chip, the combined jet system that should adopt the present invention to propose, its detailed process is: the solution of heterogeneity or suspension are under the pressure of external gas promotes, enter mixing pit from liquid storage tank by filter and pipeline, by being connected ducted solenoid control flow.Identical for guaranteeing pipeline, filter and magnetic valve to the resistance of liquid flow, should make the length of pipeline identical and degree of crook is suitable.Pipeline, filter and magnetic valve can be by proofreading and correct at the flow of different pressures and different time appointment solution or suspension to the inhibition of liquid flow, and gas pressure is controlled at 20Kp～60Kp.The design and use process of mixing pit is to the not contribution of resistance of liquid-supplying system, so the correction of solution or suspension is carried out in mixing pit or open system.The effect correction accuracy is the volatilization of liquid phase in solution or the suspension in the trimming process, so can import airtight container (as new valve bag) the back weighing quality of known quality zero volume with proofreading and correct required solution or suspension, refer to and mixing pit or the suitable environment of open system at this closed container, promptly can be to the contributive environment of liquid flowing resistance in the liquid-supplying system; Maybe will proofread and correct required solution or suspension and import weighing quality in the balance room used vapour-saturated larger volume such as the assay balance under Tc of identical liquid phase with solution or suspension.After flux modification is finished, can obtain flow and open and close the time relation curve about power air pressure and magnetic valve.Before solution or suspension mix, also should make each feed liquid pipeline that enters before the mixing pit be full of liquid and guarantee that liquid enters mixing pit simultaneously when mixing beginning, can enter mixing pit by making a small amount of heterogeneity solution or suspension much smaller than the mixing pit volume in advance, unnecessary waste liquid arrives the purpose that enters synchronously in the mixing pit by cleaning again.The design that mixing pit access pipeline distributes enters when promptly having guaranteed heterogeneity, has guaranteed that again cleaning process can not pollute liquid-supplying system.Solution or suspension enter mixing pit according to design proportion, the mixing striker that is arranged in the inlet place makes the solution or the suspension that enter mixing pit carry out first step mixing with the dispersion of droplet form and at mixing pit, start mixing pump, make solution or suspension at mixing pit and connect in the pipeline of mixing pump circulation and enter mixing pit from initial inlet, and mix by mixing the striker atomizing once more, can obtain well-mixed solution or suspension through certain hour.The solution or the suspension that mix by design spray by the electromagnetism shower nozzle.Spraying power provides gas pressure to realize by three-way magnetic valve by air inlet pipe, and electromagnetism shower nozzle emitted dose is opened and closed the rheological behavior decision of time and mixed solution or suspension by power air pressure, electromagnetism shower nozzle.Need in the use course of injection of electromagnetism shower nozzle is proofreaied and correct, proofread and correct and in open system, carry out.The effect correction accuracy is the volatilization of liquid phase in solution or the suspension in the trimming process, so can proofread and correct the well-mixed solution of ejection or closed container (as new valve bag) the back weighing quality that suspension imports the known quality zero volume, the airtight container of this zero volume promptly refer to not can be to course of injection in the contributive environment of liquid flowing resistance; Maybe will proofread and correct the well-mixed solution of ejection or suspension and import weighing quality in the balance room used vapour-saturated larger volume such as the assay balance under Tc of identical liquid phase with solution or suspension.After the electromagnetism shower nozzle is proofreaied and correct and finished, can obtain emitted dose and open and close the time relation curve about power air pressure and electromagnetism shower nozzle.The electromagnetism shower nozzle switching time has two kinds, the one, the intrinsic working time of electromagnetism shower nozzle, controlled by shower nozzle circuit and frame for movement, the one, running time, promptly refer to normally to spray the time of solution or suspension, different for the solution or the suspension of different rheological properties.Timing will be noted distinguishing.Be limited under the switching time of magnetic valve (intrinsic working time) and be limited to infinite (decision according to actual needs) on 0.18 millisecond, the drop (as 100) of the correction palpus some of emitted dose is to eliminate the accidental error of electromagnetism shower nozzle.After to hybrid electromagnetic valve and electromagnetism shower nozzle correction end, the operation cleaning procedure cleans mixing pit and electromagnetism shower nozzle.On supervisory keyboard, set switching time, electric platforms X, the step pitch of Y direction and the opening time of step number and electromagnetism shower nozzle of different component magnetic valve then successively, operation mixing jetting program.Withdraw from after moving cleaning procedure once more after finishing.The workflow of combined jet system is referring to shown in the accompanying drawing 10.
After injection is finished,, just can adopt conventional method to remove liquid phase and high temperature sintering, to form required material sample storehouse for the The parallel combined sample library.The method of removing solvent should be according to the concrete solvent decision of using (as routine techniques).High temperature sintering also is a routine techniques, should determine the temperature or the time of sintering according to the concrete kind of material.For plane and the three-dimensional device that dot matrix constitutes, after having sprayed, each layer carry out dryness finalization according to need so that the post-injection operation.Dry run can realize by two kinds of diverse ways: the one, and substrate placed on the heatable platform dot matrix that sprays is carried out real-time drying, promptly dry simultaneously in the process of spraying; The one, the substrate that injection is finished moves to and carries out retracting after drying is handled platform in the drying equipment (as baking oven) again and carry out the post-injection operation.Two kinds of methods cut both ways, and preceding method polarization and good reproducibility may produce unpredictable influence to the accurate work of magnetic valve but heating element heater can produce certain electromagnetic interference; Simultaneously, under the shower nozzle situation nearer,, the variation of shower nozzle environment temperature produces deviation with calibration curve thereby may influencing the rheological behavior of solution or suspension apart from substrate.The heat drying process can not exert an influence to course of injection in the aftermentioned method, is that certain influence is arranged but move the back at substrate to the repeatability and the accurate location of spraying.Select two kinds of different drying modes to decide according to concrete situation.
The present invention relates to a kind of method and employed electromagnetic spray system that is used to prepare combined material chip, it is characterized in that utilizing liquid injection system that DDGS solution or indissoluble thing suspension are ejected into the substrate relevant position, by appropriate heat treatment, form material chip.Be used to realize to prepare and prepare the parallel synthesizer in material sample storehouse when the DDGS solution of combined material chip or indissoluble thing suspension spraying system belong to the combined sorting new material.External gas is as power, and by the different opening times of control magnetic valve, the viscosity of binding soln or suspension is fully mixed the back and obtain the different samples of forming in mixing pit under the driving of electromagnetic pump, sprayed by the electromagnetism shower nozzle; The electromagnetism shower nozzle is fixed on the shower nozzle crane, and shower nozzle is regulated by the shower nozzle crane with respect to the height of substrate; Substrate is fixed on the two-dimentional X-Y electric platforms, two dimension electric platforms horizontal positioned, shower nozzle crane and two-dimentional electric platforms are fixed on same workbench, and single-chip microcomputer drives two-dimentional electric platforms by the controller of electric platforms, the switching of the control driver control magnetic valve by magnetic valve.
Description of drawings
Fig. 1 is the spraying system structural representation
Fig. 2 is the hybrid chamber structural representation
Fig. 3 is the circuit theory of electromagnetic spray system
Fig. 4 is single chip circuit and pin function signal
Fig. 5 is LCD pin function and peripheral circuit
Fig. 6 is each the key function signal of five key boards
Fig. 7 is a driving circuit for electromagnetic valve
Fig. 8 is the input waveform (a) and the output waveform (b) of drive circuit
Fig. 9 is three power supplies of Circuits System
Figure 10 is the workflow of combined jet system
The specific embodiment
Below by the elaboration of specific embodiment, to further specify substantive distinguishing features of the present invention and obvious improvement.
Embodiment 1 electromagnetic spray system provided by the invention is made up of pipe-line system and navigation system
The pipe-line system of described spraying system is made of gas piping, liquid line, flow-control magnetic valve and hybrid electromagnetic pump.Gas piping is by sample air inlet pipe, injection air inlet pipe and cleaning fluid air inlet pipe (9-A ,-B ,-C as shown in Figure 1, ... ,-J ,-S) form, sample air inlet pipe (9-A ,-B ,-C wherein, ...) and liquid storage tank (7-A,-B ,-C ...) link to each other, spray air inlet pipe (9-J) and link to each other with mixing pit (3), cleaning fluid air inlet pipe (9-S) links to each other with cleaning liquid pool (7-S).Fluid pipeline is by liquid storage tank (7-A ,-B ,-C, ...), sample feed tube (8-A ,-B ,-C, ...), the connecting pipe (2-T) of mixing pit (3), electromagnetic pump (2) and mixing pit (3), clean liquid pool (7-S) and form, liquid storage tank (7-A ,-B wherein,-C ...) by sample feed tube (8-A ,-B,-C, ...) be connected with mixing pit (3), electromagnetic pump (2) is connected with mixing pit (3) by connecting pipe (2-T), cleans liquid pool (7-S) and is connected with mixing pit (3).The flow-control magnetic valve by with sample feed tube (8-A,-B,-C ...) the sample magnetic valve (the 4-A ,-B that connect,-C, ...), the cleaning fluid magnetic valve (5) that is connected with cleaning fluid feed tube (8-S), the electromagnetic pump (2) that is connected by connecting pipe (2-T) with mixing pit (3), with the three-way magnetic valve (6) that injection air inlet pipe (9-J) is connected, the electromagnetism shower nozzle (1) that is connected with mixing pit (3) is formed.Admission line, liquid storage tank, sample feed tube etc. are according to the first number decision of the chip of preparation.At least be A, B binary system, but as many as is infinitely individual in theory, becomes but be generally ternary, quaternary or five-tuple.
The solution of required DDGS or the suspension of indissoluble thing are mixed in hybrid chamber according to different proportionings, at the desired location metered injection, preparation material chip, the combined jet system that should adopt the present invention to propose.
The injection navigation system of described spraying system is made up of two-dimentional X-Y electric platforms (11,12) and electric platforms control system (15).Wherein mixing pit (3) and electromagnetism shower nozzle (1) are fixed in two-dimentional X-Y electric platforms (11 by shower nozzle crane (10), 12) on, backing plate (13) is fixed in two-dimentional X-Y electric platforms (11,12) on, two dimension X-Y electric platforms (11,12) is driven by electric platforms controller (15) by control single chip computer (14).
The DDGS solution of material chip of the present invention or indissoluble suspension spraying system, use characteristic is under external gas pressure drives, Pneumatic pipe cleaner is crossed sample air inlet pipe (9-A,-B,-C, ...) promotion liquid storage tank (7-A,-B,-C, ...) in DDGS solution or indissoluble thing suspension by sample feed tube (8-A ,-B ,-C, ...) enter mixing pit (3), utilize and sample feed tube (8-A ,-B ,-C, ...) the sample magnetic valve (4-A that connects,-B ,-C ...) and open and close controlling enter the different solutions of mixing pit (3) or the amount of suspension, mix by electromagnetic pump (2) and with the solution or the suspension of mixing pit connecting pipe (2-T), provide gas pressure to promote solution or suspension process electromagnetism shower nozzle (1) ejection in the mixing pit (3) by spraying air inlet pipe (9-J) by three-way magnetic valve (6) to mixing pit (3); Cleaning fluid enters mixing pit (3) through cleaning fluid feed tube (8-S) in air inlet pipe (9-S) the promotion cleaning liquid pool (7-S) by cleaning, start electromagnetic pump (2) clean electromagnetic pump and with the mixing pit connecting pipe, clean waste liquid and provide ejection under the gas pressure at three-way magnetic valve (6), clean electromagnetism shower nozzle (1) simultaneously by electromagnetism shower nozzle (1).Electromagnetism shower nozzle (1) is fixed on the shower nozzle crane (10), and electromagnetism shower nozzle (1) is regulated by shower nozzle crane (10) with respect to the height of substrate (13); Substrate (13) is fixed on two-dimentional X-Y electric platforms (11,12) on, two dimension X-Y electric platforms (11,12) horizontal positioned, shower nozzle crane (10) and two-dimentional X-Y electric platforms (11,12) be fixed on the same workbench, control single chip computer (14) is by the two-dimentional X-Y electric platforms of controller (15) (11,12) of electric platforms, by magnetic valve (4,5) three-way magnetic valve (6), electromagnetic pump (2), control driver element (16) control of electromagnetism shower nozzle (1) drives magnetic valve (4,5), three-way magnetic valve (6), electromagnetic pump (2), the switching of electromagnetism shower nozzle (1).
Described mixing pit (3) mixes striker (18) and pipe joint (19-1 ,-2 ,-3 ,-4 by mixing chamber (17), ...) form, mixing chamber (17) is cylindrical, mixes striker (18) and is positioned at pipe joint (19-1,-2 ,-3 ...) liquid outlet, pipe joint (19-1 ,-2 ,-3,-4 ...) and feed tube (8-A ,-B,-C ... ,-S), air inlet pipe (9), electromagnetic pump (2) be connected with electromagnetism shower nozzle (1) with mixing pit connecting pipe (2-T).Specifically see also accompanying drawing 2.
The preparation method of DDGS solution: with Ga (spectroscopic pure), Y
2O
3(analyzing pure), Tb
4O
7(analyzing pure), Eu
2O
3(analyzing pure), nitric acid are complexing agent as raw material with the citric acid, and fixedly the ratio of citric acid and metal ion total amount is 1.5: 1.Oxide is dissolved in respectively in an amount of nitric acid, is that complexing agent network and metal ion form the transparent solution of stable uniform with the citric acid.
Spraying system is a ternary component, and getting A is Ga
3+-citric, B are Y
3+-citric, C are Tb
3+Or Eu
3+-citric.Get A: B: the ratio of C is 5: 3 (1-x): 3x (in metal ion), wherein x=0.01,0.015,0.020,0.025 and 0.030.
After required solution mixed in hybrid chamber according to different proportionings, at the desired location metered injection, the preparation material chip, the combined jet system that should adopt the present invention to propose, its detailed process is: the complex solution of different metal citrates is under the pressure of external gas promotes, enter mixing pit from liquid storage tank by filter and pipeline, by being connected ducted solenoid control flow.Identical for guaranteeing pipeline, filter and magnetic valve to the resistance of liquid flow, should make the length of pipeline identical and degree of crook is suitable.Pipeline, filter and magnetic valve can be proofreaied and correct at the flow of different pressures and different time by the complex solution to the specified metal citric acid the inhibition of liquid flow, and gas pressure is controlled at 20Kp～60Kp.The correction of the complex solution of metal citrate is carried out in mixing pit or open system.The effect correction accuracy is the volatilization of liquid phase in the solution in the trimming process, so can import airtight container (as new valve bag) the back weighing quality of known quality zero volume with proofreading and correct required solution, refer to and mixing pit or the suitable environment of open system at this closed container, promptly can be to the contributive environment of liquid flowing resistance in the liquid-supplying system; Maybe will proofread and correct required solution and import weighing quality in the balance room that has used vapour-saturated larger volume such as the assay balance under Tc of identical liquid phase with solution or suspension.After flux modification is finished, can obtain flow and open and close the time relation curve about power air pressure and magnetic valve.Before the complex solution of metal citrate mixes, also should make each feed liquid pipeline that enters before the mixing pit be full of liquid and guarantee that liquid enters mixing pit simultaneously when mixing beginning, can enter mixing pit by making a small amount of heterogeneity solution much smaller than the mixing pit volume in advance, unnecessary waste liquid arrives the purpose that enters synchronously in the mixing pit by cleaning again.The design that mixing pit access pipeline distributes enters when promptly having guaranteed heterogeneity, has guaranteed that again cleaning process can not pollute liquid-supplying system.The complex solution of metal citrate enters mixing pit according to design proportion, the mixing striker that is arranged in the inlet place makes the solution or the suspension that enter mixing pit carry out first step mixing with the dispersion of droplet form and at mixing pit, start mixing pump, make the complex solution of metal citrate at mixing pit and connect in the pipeline of mixing pump circulation and enter mixing pit from initial inlet, and mix by mixing the striker atomizing once more, can obtain the complex solution of well-mixed metal citrate through certain hour.The solution or the suspension that mix by design spray by the electromagnetism shower nozzle.Spraying power provides gas pressure to realize by three-way magnetic valve by air inlet pipe, and electromagnetism shower nozzle emitted dose is opened and closed the rheological behavior decision of time and mixed solution by power air pressure, electromagnetism shower nozzle.Need in the use course of injection of electromagnetism shower nozzle is proofreaied and correct, proofread and correct and in open system, carry out.The effect correction accuracy is the volatilization of liquid phase in the solution in the trimming process, so can proofread and correct closed container (as new valve bag) the back weighing quality that the well-mixed solution of ejection imports the known quality zero volume, the airtight container of this zero volume promptly refer to not can be to course of injection in the contributive environment of liquid flowing resistance; The well-mixed solution that maybe will proofread and correct ejection imports weighing quality in the balance room that has used vapour-saturated larger volume such as the assay balance under Tc of identical liquid phase with solution.After the electromagnetism shower nozzle is proofreaied and correct and finished, can obtain emitted dose and open and close the time relation curve about power air pressure and electromagnetism shower nozzle.The electromagnetism shower nozzle switching time has two kinds, and the one, the intrinsic working time of electromagnetism shower nozzle, controlled by shower nozzle circuit and frame for movement, the one, running time promptly refers to normally to spray time of solution, and is different for the solution of different rheological properties.Timing will be noted distinguishing.The drop (as 100) of the correction palpus some of emitted dose is to eliminate the accidental error of electromagnetism shower nozzle.After to hybrid electromagnetic valve and electromagnetism shower nozzle correction end, the operation cleaning procedure cleans mixing pit and electromagnetism shower nozzle.On supervisory keyboard, set switching time, electric platforms X, the step pitch of Y direction and the opening time of step number and electromagnetism shower nozzle of different component magnetic valve then successively, operation mixing jetting program.Obtain design Eu
3+, Tb
3+The Y that mixes
3Ga
5O
12Combined material chip, withdraw from after moving cleaning procedure once more after finishing.
After injection is finished,, just can adopt conventional method to remove liquid phase and high-temperature process, to form required material chip for the mixed solution sample on the substrate.The method of removing solvent should be according to the concrete solvent decision of using (as routine techniques).High-temperature process also is a routine techniques, should determine the temperature or the time of sintering according to the concrete kind of material.The present embodiment sample promptly obtains the material requested chip 800 ℃ of following heat treatments 2 hours.
The preparation method of indissoluble thing suspension: with Ga
2O
3(analyzing pure) Y
2O
3(analyzing pure) Tb
4O
7(analyzing pure) Eu
2O
3(analyzing pure) as dispersant, selects the QM-1SP planetary ball mill of Nanjing Univ. Instrument Factory's production with PAA (Mw=45k) for use as raw material.Ball milling condition: with raw material, dispersant and deionized water are put into ball grinder with 1: 0.02: 9 ratio, again the agate ball of diameter 10mm and 6mm suitably after the collocation, is put into ball grinder together in 10: 1 ratio of ratio of grinding media to material, sealing is afterwards with 250 rev/mins rotating speed ball milling 20 hours.Promptly get the suspension that needs, these suspension can not produce sedimentation in the long period under dispersant stable.
Spraying system is a ternary component, and getting A is Ga
2O
3, B is Y
2O
3, C is Tb
4O
7Or Eu
2O
3Get A: B: the ratio of C is 5: 3 (1-x): 3x (in metal simple-substance), x=0.01 wherein, 0.015,0.020,0.025,0.030.
By the detailed process of suspension preparation material chip referring to embodiment one.High-temperature heat treatment process is different, is 1150 ℃ and is incubated 4 hours down.
Claims (10)
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100423227A CN101342525A (en) | 2008-08-29 | 2008-08-29 | Method for preparing combined material chip and electromagnetic injection system used |
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|---|---|---|---|
| CNA2008100423227A CN101342525A (en) | 2008-08-29 | 2008-08-29 | Method for preparing combined material chip and electromagnetic injection system used |
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|---|---|
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Family
ID=40244716
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105449188A (en) * | 2015-01-04 | 2016-03-30 | 宁波英飞迈材料科技有限公司 | Cathode composite material chip for lithium-ion battery and preparation method |
| CN107694796A (en) * | 2017-10-18 | 2018-02-16 | 浙江丰诚智能科技有限公司 | A kind of full-automatic heat forges manufacture system inkjet mechanism |
| CN118437534A (en) * | 2024-07-08 | 2024-08-06 | 烟台奥森制动材料有限公司 | Spraying mechanism for carbon fiber composite material laminating equipment |
-
2008
- 2008-08-29 CN CNA2008100423227A patent/CN101342525A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105449188A (en) * | 2015-01-04 | 2016-03-30 | 宁波英飞迈材料科技有限公司 | Cathode composite material chip for lithium-ion battery and preparation method |
| CN107694796A (en) * | 2017-10-18 | 2018-02-16 | 浙江丰诚智能科技有限公司 | A kind of full-automatic heat forges manufacture system inkjet mechanism |
| CN118437534A (en) * | 2024-07-08 | 2024-08-06 | 烟台奥森制动材料有限公司 | Spraying mechanism for carbon fiber composite material laminating equipment |
| CN118437534B (en) * | 2024-07-08 | 2024-08-27 | 烟台奥森制动材料有限公司 | Spraying mechanism for carbon fiber composite material laminating equipment |
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Open date: 20090114 |