CN101522314A - Film formation and evaluation - Google Patents
Film formation and evaluation Download PDFInfo
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- CN101522314A CN101522314A CNA2007800275816A CN200780027581A CN101522314A CN 101522314 A CN101522314 A CN 101522314A CN A2007800275816 A CNA2007800275816 A CN A2007800275816A CN 200780027581 A CN200780027581 A CN 200780027581A CN 101522314 A CN101522314 A CN 101522314A
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Abstract
Methods and apparatus for forming films from liquid samples for evaluation are disclosed. The liquid samples are dispensed into a channel formed by a die and a substrate on which the films are generated whilst moving the die and the substrate relatively to one another. Once formed, the liquid films may then be further processed, for example by curing or polymerisation, to generate solid films for subsequent evaluation.
Description
The present invention relates on the surface of substrate (substrate) to form film and to the evaluation of the characteristic of such film.
Coating (coating) be widely used in industry with the environment of family expenses in, increasing the functional and added value of bulk material and article, and the outward appearance of improving structure.Other application comprises non-continuous coating, such as printing ink.Organic coating is widely used in many industrial protection/decorative applications especially; for example the automobile face be coated with clear coat, automobile with and decoration is painted and lacquer (lacquer), colored paint and do not have colored paint; for example priming paint, bottoming and finish paint paint system etc., and organic coating also is used in the printing ink.The organic coating of other type comprises for example protection and corrosion-inhibiting coating, bonding and anti-stick coating, environmental barrier coating (environmental barrier coating), conduction/transparent coatings and scratch resistant hard conating (scratchresistant hard coating).Coating although it is so can only be made up of organic component, but other coating can comprise inorganic constituents, for example metal oxide pigment, conducting metal particles, inorganic particles packing, such as the clay of vermiculite, and the inorganic particle of similarly knowing.
The inorganic coating that also has the many forms to comprise organic adhesive or selectively can form by aqueous dispersion.The inorganic coating of other form can be applied directly to substrate with coating material by the technology by use such as spraying and vapor deposition (deposition) chemistry or physics and form.
In food and other application, food or other material are formed the purpose of film to be used to test or compare, also may be useful.Can be tested or such food relatively and other material are, for example, dough/pasta, starch film, sauce (sauces), mustard and analog, and in personal care applications, be toothpaste, shaving cream and analog.
To the new combination of the component of coating material or new processing conditions carries out especially fast and the test of large sample to find material of future generation or ability new, cost-effective manufacture method, on the agenda of many manufacturers, be important, so that they can obtain to surmount competitor's commercial advantage.What have tangible importance equally is the ability with performance drift (performance drift) of the existing preparation of test, when especially working as the component that substitutes selectable component or can select to originate.
Above-mentioned hope can be applicable to other material such as structural material equally more at large, especially when at least some performances in the performance of being concerned about of such material can be measured by the membrane sample of such material.
In addition, produce the material be used to test or be used to make with multilayer be concerned about.The example of such multilayer material comprises: use the multilayer of different adhesives for example to adhere to produce between the substrate with different surfaces energy, and produce different adhesion properties thus; Priming paint, bottoming and finish paint paint system; With the semiconductor device of multilayer, the overall performance of wherein such device not only highly depends on the intrinsic property of the constituent material in each layer, but also depends on concrete stacked order, interface and the surface texture of adding that uses in preparing such device.
There has been the trial that produces and test the wide variety of materials sample, for example disclosed among US 6482264 B1, US 2003/0224105 A1, US 2004/0071888 A1 and DE 10136448 A1.These publications disclose and have deposited and be coated with sample to form the several different methods of film in substrate, in certain methods, comprise: use such as the noncontact method of rotation or concussion substrate and come the coating liquid sample, perhaps use air knife to come the coating liquid sample, perhaps liquid sample is ejected in the substrate.In preparation self-adhesive tape (self-adhesive tape) or sheet, binder deposition also is known and is described among the GB 916406 to base band (backing tape).
The shortcoming that these methods exist is, owing to be deposited on suprabasil small amount of liquid, the uniformity of formed film can change significantly, thereby and the parameter of being surveyed may not be determined exactly.Though this is for some materials or for shielding material, for example based on by/by (pass/fail), may not be important, it may be crucial in other is used.For example, in the colour specification of measuring paint, lacquer, printing ink etc., the thickness of film and uniformity may influence the colour measurement process significantly.In addition, the amount that sample stands to shear during being coated with may influence the dispersion of granules of pigments, and influences the uniformity of the gained color of membrane sample thus.
Be used to form the film that is used to test, in particular for form can stand resistivity measurement or be known for other technology of the film that in such as dynamic mechanics heat analysis (dynamic mechanical thermal analysis) mechanical test (DMTA), uses.Such technology is made up of following: the adhesive tape by will having known thickness with selected interval be applied in parallel with each other the substrate of microslide for example or easily with film from its substrate of peeling off, in this substrate, form passage with specified width, which width and degree of depth; Liquid sample is deposited in the passage; With the upper surface that scraping blade (doctor blade) is pulled through described band, to remove excess liquid from being formed on suprabasil passage.Yet these technology are time-consuming, when having a plurality of samples of same or similar composition especially if desired or will prepare the sample with multilayer material.
The objective of the invention is to reduce or eliminate at least a shortcoming in the aforesaid drawbacks.
According to a first aspect of the invention, the method that forms film on the surface of substrate comprises: provide and hold the container of the sample position location on substrate surface (sample location position) being located to form the liquid sample of film, described container has the outlet that comprises die head (die), described die head has tabular surface (planar face), described tabular surface can contact with described substrate, defines the passage that is used for receiving from described container at least a portion of described liquid sample with this; Described die head is contacted with the end place of described substrate in described sample position location; Make described liquid sample extrude and enter described passage by described die head, simultaneously, described die head and described substrate are moved each other in contact and relatively, described thus die head moves towards the far-end of described sample position location, with the film at the described liquid sample of place, described sample position location deposition.
Though in four corner of the present invention, as long as pressure can be applied to liquid sample in the container, container just can be the shape that is fit to arbitrarily; But in preferred embodiments, described container has general cylinder form, and a piston mobile is wherein arranged.In particularly preferred embodiments, described container is the commercial tube of buying, for example can be from the plastic injector of EFD acquisition.Usually, described tube or syringe can have scope at 5ml to 100ml, the volume in the 5ml to 50ml more preferably, and have the volume of 10ml usually.
Preferably, syringe seals with cap in its exit, and described cap is dismountablely to allow described die head to be coupled to this syringe.Preferably, described die head has the protuberance of annular on the opposite side of described tabular surface, and this protuberance replaces described cap sucking fit (push fit) on the exit portion of syringe.The protuberance of annular defines the part by the path of described die head, can extrude liquid sample from container by described die head.
In the method for the invention, described liquid sample can flow through die head under the capillarity of described liquid sample, to contact with described substrate at place, described sample position location.Selectively, perhaps possibly,,, described liquid sample make described liquid sample flow through die head by being exerted pressure with the capillarity combination.
Preferably, this method comprises: pressure is applied to described liquid sample in the container, so that described liquid sample flow to the main volume (prime volume) that is enough to fill in the described die head.
In a preferred embodiment of the invention, described method comprises: form described passage by the notch (rebate) that described path leads to wherein is provided in the tabular surface of described die head.
In one embodiment, described notch fully longitudinally extends through the opposite end of the tabular surface of described die head up to described die head, to form opening thus.
In selectable embodiment, described notch preferably only partly longitudinally extends through the tabular surface of described die head, extends to an end of described die head at least from described path, to form opening thus.In this example, described method comprises: described die head and described substrate are movable relative to each other, so that the die end that described opening is positioned at wherein is in afterbody with respect to the direction that relatively moves of described die head.Preferably, described notch extends beyond the distance of one section weak point of described path towards the opposite end of described die head, forms dead space (dead space) thus.
In another selectable embodiment, described method comprises: by providing groove (groove) to form described passage at place, described sample location in described substrate, form described passage thus when described die head contacts with described substrate at a described end place of described sample position location.Preferably, described groove has predetermined length.
In the further selectable embodiment of another kind, described method comprises: form described passage by the foregoing groove that is positioned at place, described sample location in foregoing notch in the tabular surface that described die head is provided and the described substrate, thus, when described die head contacted at a described end place of described sample position location with described substrate, described notch formed described passage with described groove.
In the described in front embodiment, preferably, notch and/or groove have predetermined cross section.
In the preferred embodiment of the invention, the tabular surface of described die head is flat.Yet, be susceptible to, form along its length be curve film also within the scope of the invention, in this example, the tabular surface of substrate and described die head can be arc, and is complimentary to one another on its direction that relatively moves.
In case described the relatively moving by die head and substrate deposited film, just stop the described liquid sample in the container is exerted pressure, and die head is removed from substrate.
Should be understood that when method utilization of the present invention has the die head of notch this method depends on the dynamic viscosity (dynamic viscosity) of institute's deposited liquid sample, to keep film shape or cross section.Therefore, when utilizing such die head, liquid will need dynamic viscosity, so that it keeps film shape or cross section.Usually, use the liquid-like that has in the about dynamic viscosity of 0.05Pa.s in the scope of about 100Pa.s to form film originally.
Yet the surface energy round the sample position location at the bottom of the adjustable integral basis is to allow that use has the liquid-like that is lower than about 0.05Pa.s dynamic viscosity and formed film originally.
In addition, when method utilization of the present invention formed the substrate of groove therein, by the liquid sample with low dynamic viscosity, it also was possible that the liquid-like that for example has a dynamic viscosity that is lower than about 0.05Pa.s formed film originally.
If form arc film, so significantly, the dynamic viscosity of liquid sample will be had to relatively high, so that liquid sample keeps its shape after deposition.
Being used to make die head and the contacted power of substrate normally in the scope from about 10N to about 100N, more generally is in the scope from about 15N to about 35N.
Be used for will depending on from the power that container is extruded liquid sample the dynamic viscosity of liquid sample, higher viscosity needs bigger power.Yet usually, applied force is in the scope from about 0N to about 200N, and this depends on and whether only depends on capillarity or whether applied positive force.More preferably, applied force is in the scope from about 0.1N to about 200N.
For many application, preferably, method of the present invention comprises: the film of handling the liquid sample that so forms is so that its curing.This may only relate to allows that solvent and/or current-carrying (carrier fluid) evaporate under environment temperature.Yet it can comprise makes liquid film stand freeze drying and/or heating and/or reduced pressure atmosphere, desolvates and/or current-carrying with auxiliary removing.The chemical system that depends in film to be considered, can be at environment temperature and/or environmental pressure, perhaps be below or above under environment temperature and/or the environmental pressure, and/or for example use incident radiation such as the UV radiation, perhaps pass through known in the art other technology arbitrarily, solidify and/or the polymeric liquid sample.
Method of the present invention comprises the formation film, described film comprises the composite membrane with at least two retes, by first rete being deposited in the substrate by any embodiment in the foregoing embodiment herein, and then second rete is deposited on first rete, and if desired, follow-up rete is deposited on second rete and the follow-up rete in turn, forms described composite membrane.Depend on and be used for first rete is deposited on suprabasil embodiment, promptly whether by groove with do not have a die head of notch, perhaps groove and have a die head that whether longitudinally extends the notch of its tabular surface, perhaps it makes up and defines passage, can use the die head with notch that second rete is deposited on first rete, described notch can be fully longitudinally or can not exclusively longitudinally be extended the tabular surface of die head.Can use the die head with notch that follow-up rete is deposited on and go up most on the rete, described notch fully longitudinally extends the tabular surface of die head.At least one die head with the notch that fully longitudinally extends its tabular surface can be used for forming at least one and goes up rete most, and the degree of depth of notch is greater than the thickness of the rete that is deposited outstanding on the substrate surface.
In order to make first rete and follow-up rete withstand second rete and follow-up rete deposition thereon, the rete that receives further rete must sufficiently be stablized, to keep its shape during deposition process.Such stability can be granted by the die head that supports rete during deposition process at least in part.Selectively, perhaps in addition, the rete that receives the further deposition of liquid sample can have sufficiently high dynamic viscosity to keep its shape between the depositional stage of further rete, perhaps can aforesaidly be cured.The dynamic viscosity of the rete of the further deposition of reception liquid sample can be high inherently, perhaps can bring up to enough levels so that film solidifies by using above-described technology.
Method of the present invention comprises: by film being deposited on the place, respective sample position location on the described substrate surface, come to form a plurality of films on described substrate surface, described sample position location is to have living space each other to concern.Expediently, it is no more than 100 to be distributed in described lip-deep number of samples, but can be 2 or more usually, and for example 4,8,16,32 or 64.
Preferably, the film that forms on substrate surface is discontinuous each other.
Usually, formed film or each film have width in about 150mm scope of about 1mm, about 5mm in about 50mm scope length and 20 μ m to 1000 μ m, be more typically in the degree of depth of 25 μ m in 800 mu m ranges.The size that However, it should be understood that film can be depending on application, and may be more higher or lower than the scope of being quoted from.
Though can on the surface of single substrate, form membrane array, in selectable embodiment, can on the surface of substrate array, form monofilm or multilayer film.For example, substrate can be a microslide, and has deposited monofilm thereon.Selectively, substrate can have sizable area (significant area), and has deposited the film that surpasses one deck thereon.The material of substrate can be the material of any suitable, and can be glass, metal, plastics usually.The material of substrate can have antiseized character (release quality), for example substrate of PTFE, and the film that can freely place can remove to be used for follow-up test from substrate thus.
In case the formation film is just measured at least one characteristic of film.Be not limited to following example, characteristic can be a physics, for example color, transparency, marresistance, wearing and tearing; Chemistry, environmental stability/tolerance for example; Machinery, for example intensity, modulus; Perhaps electricity, for example resistance, electric conductivity.
In particularly preferred embodiment of the present invention, the method that forms a plurality of films at lip-deep each place, sample position location of substrate comprises:
(a) provide multiple liquid sample in corresponding syringe, described syringe is at the corresponding cap closure of its port of export quilt;
(b) concurrently or preferred sequence ground, remove cap and die head is coupled to the port of export of syringe from each syringe, each described die head can contact with described substrate, defines the corresponding passage of at least a portion that is used for receiving liquid sample with this;
(c) concurrently or preferred sequence ground, corresponding described die head is contacted with the end place of described substrate in corresponding described sample position location;
(d) concurrently or preferred sequence ground, make the liquid sample in each corresponding syringe extrude and enter corresponding described passage by corresponding described die head, simultaneously, described die head and described substrate are moved each other in contact and relatively, described thus die head moves towards the far-end of described sample position location, with the film at the described liquid sample of place, described sample position location deposition.
Allow as context, foregoing feature of the present invention is applied in this particularly preferred embodiment of the present invention with having done necessary correction.
Preferably, method of the present invention comprises the step that removes die head and syringe is blocked a shot again from syringe.
The present invention also comprises the equipment that can implement the inventive method by it.
More specifically, according to a second aspect of the invention, the equipment that is used for formation film on the surface of substrate comprises substrate support device and distribution system (dispensing system), described distribution system is used in the operating period of described equipment at least a liquid sample being distributed in the place, lip-deep sample position location of the substrate of being supported by described substrate support device, described distribution system comprises the clamping device (gripper means) that is used for fixing container, in use, described container receiving fluids sample, described container has the outlet that comprises die head, described die head has tabular surface, this tabular surface can contact with described substrate, define the passage that is used for receiving at least a portion of described liquid sample with this from described container, described distribution system can be operated described die head is contacted with the end place of described substrate in described sample position location, simultaneously, described distribution system side by side can be operated basically described die head and described substrate are moved each other in contact and relatively, described thus die head moves towards the far-end of described sample position location, with the film at the described liquid sample of place, described sample position location deposition.
Allow as context, the front is applied to according in the equipment of the present invention in conjunction with the described apparatus characteristic of method of the present invention with having done necessary correction.
Preferably, described distribution system comprises the device that the liquid sample in the described container is exerted pressure.
Preferably, distribution system comprises the piston rod that can engage with the piston in the described container, and described thus piston is removable to be realized the positive displacement (positivedisplacement) of the described liquid sample in the described container or retreat (drawback).Preferably, by preferably include be connected to described piston rod, by for example drive unit of stepping motor driven lead screw (motive means), described piston rod can move with respect to described clamping device.Preferably, motor is can be from the MDrive stepping motor of IMS USA acquisition, and it provides the linear resolution of 1 μ m.
Preferably, described piston rod can engage with described piston by second clamping device.Second clamping device preferably includes at least one that can move, two clampers more preferably between non-moving position (inactive position) and moving position (activeposition), engage described piston at clamper described in the described moving position or each clamper.Preferably, described clamper or each clamper comprise spring steel and have engage with described piston radially outward towards barb.
Preferably, described piston rod is a hollow, and the radially line of rabbet joint (diametral slot) with the part of extending its length from its lower end, this clamper or each clamper are installed as near described lower end, and opposed half (opposed half) passing through the described lower end of piston rod moves against its radially outer of natural elasticity, this clamper or each clamper can move to described moving position radially outwardly, and by opposed half radially inner moving under its natural elasticity of piston rod, this clamper or each clamper turn back to described non-moving position.Preferably, by having bellend and being installed to the axial displacement (axial displacement) that is used in the described piston rod relative to its central component that moves, for example use pneumatic actuator, realize opposed half the moving radially of described piston rod.
Equipment of the present invention comprises automation processing equipment, described automation is handled equipment and is used for index described substrate support device respect to one another and described distribution system, thus in use, can on the substrate surface at least two films be deposited on the place, sample position location that has living space each other on the described surface and concern.
Method and apparatus of the present invention also comprise may be below feature as described in conjunction with the accompanying drawings.
The present invention is also included within described die head herein.Die head can be made by the material of any suitable.For example, die head can be made by plastics or metal.In arbitrary example, depend on the character of liquid sample and the material of die head, die head can discard, and perhaps preferably uses solvent or other clean method to clean to be used for follow-up re-using.
Preferably, the path by die head ends at the line of rabbet joint that extends transverse to die head usually.Preferably, the line of rabbet joint extends through the whole width of described passage basically, and described passage can be defined between the corresponding substrate that described die head and described die head will therewith use.
As discussing ground in the early time, coating can be made by various materials, and in context of the present invention, can prepare film by organic material and inorganic material, and condition is that material is liquid form or solution or is scattered in the liquid-carrier.Typical application comprises adhesive, polymer, resin, paint, printing ink, metallic solution, starch, the dispersion that comprises nanoparticle dispersion, multi-lager semiconductor material etc.In many such application, material can be conduction or nonconducting.
The present invention also comprises at least one membrane array, more preferably is to comprise at least two membrane arrays and each described membrane array all in suprabasil film storehouse, and wherein each film sample for reference position location is positioned evenly in the array.
Set forth the present invention now with reference to accompanying drawing and the following example.In the accompanying drawings:
Fig. 1 is the schematic plan view according to equipment of the present invention;
Fig. 2 is the schematic side elevation of biopsy cavity marker devices of the distribution system of the equipment shown in Fig. 1;
Fig. 3 A to Fig. 3 C is respectively the cross-sectional view along A-A line among Fig. 3 C of the die head that uses in method and apparatus of the present invention, along the cross-sectional view of B-B line among Fig. 3 A with along the elevation of arrow C among Fig. 3 A;
Fig. 4 is the schematic vertical cross-section by the lower end of the piston rod shown in Fig. 2 86;
Fig. 5 is the syringe cap of Fig. 1 and the schematic side elevational elevation that die head removes the biopsy cavity marker devices of platform (die removal station) 32;
Fig. 6 A to Fig. 6 C is respectively the cross-sectional view along A-A line among Fig. 6 C of the another embodiment of the die head that uses in method and apparatus of the present invention, along the cross-sectional view of B-B line among Fig. 6 A with along the elevation of arrow C among Fig. 6 A; And
Fig. 7 and Fig. 8 are the MIcrosope images of the composite membrane that dissects described in following examples 3 and embodiment 4.
Stand (rack) 18, it holds syringe 20, for example can be from the 10ml syringe of EFD acquisition;
Two stands 22, for example 32 slide (not shown) can be installed in each stand 22 securely, when use equipment 10, liquid film can be deposited on each slide, each stand has upper plate (as directed), upper plate have corresponding to but the elongated line of rabbet joint 24 of sample position location on the corresponding slide;
Syringe cap and die head remove platform 32;
The receiving vessel (not shown), it can hold solvent or other liquid, and it is arranged in the below in the hole of base plate 16, is used for receiving syringe cap 36 and the die head 30 that is removed;
The receiving vessel (not shown), it is arranged in the below in the hole of base plate 16, is used for receiving used syringe 20; And
Distribution system 34 (seeing Fig. 2), it is installed on the treatment system 14, is used for vertically moving (Z axis) with respect to framework 12.
Although slide has been illustrated as the substrate for the film of receiving liquid sample body, should be understood that by the description that starts other material and other big or small substrate can be easily with equipment 10 uses of the present invention.
According to the present invention, die head 30 (seeing Fig. 3 A to Fig. 3 C) can by plastics or for example the metal-made of brass get, and each die head has elongate body (elongate body) 40, in the present embodiment, elongate body 40 has round nose 42, round nose 44 and is centrally located on annular protuberance 46 on its upper surface, and annular protuberance 46 is coaxial with cylinder hole (the cylindrical hole) 48 in the main body 40. The annular protuberance 46 the upper end in 47 places by reaming, with the port of export of auxiliary positioning syringe 20.
Be processed with or be molded with notch 54 in the lower flat surfaces of the main body 40 of die head 30 (planar surface) 52, notch 54 be opened on main body 40 an end 42 and from this end 42 towards the opposite end 44 longitudinal extensions more than the amount of half length of main body 40, it ends at the position above the line of rabbet joint 50 thus, so that liquid dead space 56 to be provided. If be considered as little liquid container to regulate little pressure oscillation and auxiliary surface is wetting possibly, it is preferred that such dead space 56 then is provided. The size of notch 54 will be shaped to the film that can produce required size as previously described.
Syringe cap and die head remove platform 32 and have chock on first (upper wedge) 60, this on first chock 60 have U-shaped hole 62 be used to the lower end that holds the syringe 20 that is carried by distribution system 34 (being illustrated with cap 36), those parts at the edge (limb) in the formation hole 62 of chock 60 abut against fully together to engage cap to be removed 36 or die head 30. 62 openend is tapered the first chock 60 towards the hole, and has the upper surface of horizontal alignment and the lower surface of inclination, and is installed on bearing (bearing) (not shown), is used for as arrow is indicated does back and forth vertical movement. Platform 32 also has the second chock 64, the second chocks 64, and to have U-shaped hole 66, the second chocks 64 substantially the same with the first chock 60, but compare with the orientation of the first chock 60, has inverted orientation. The second chock 64 is installed on the pneumatic actuator (not shown), moves horizontally for doing back and forth such as the indicated XY orientation with respect to the first chock 60 of arrow. The second chock 64 makes the lower horizontal surface of the second chock 64 engage cap 36 (or die head 30) and the first chock 60 be moved so that cap 36 (or die head 30) separates with syringe 20 together with distribution system 34 towards the movement of the first chock 60.
For vertical movement, being installed on the driving screw 84 is hollow piston rod 86, and being installed in hollow piston rod 86 lower ends is spreader member 88, and spreader member 88 can move axially along piston rod 86. What be installed in equally piston rod 86 lower ends is the spring steel clamping device 90 of two diametrically contrapositions, and spring steel clamping device 90 has little barb (slight barb) 92 at its lower end. The lower end that upwards the moving axially of member 88 makes clamper 90 is radially outwards mobile and engage piston head member (not shown) in the syringe 20, simultaneously, this reverse movement of moving so that clamper 90 because its intrinsic elasticity and radially inwardly return and break away from such piston component.
In operation, distribution system 34 processed systems 14 move to stand 18 and obtain the first syringe 20. Because the volume of the material in the syringe 20 is unknown, before clamper 80 clamping syringes 20, use motor 82 and driving screw 84 that piston rod 86 is dropped in the syringe 20, until sense moving up of distribution system 34 owing to contacting with piston head member in the syringe 20. After sensing such movement, stop the movement of piston rod 86, and piston rod 86 is moved down by the amount that the user determines, so that the upper liquid from syringe 20 of die head perfusion. Then clamper 80 is drawn close with clamping syringe 20.
Then distribution system 34 is moved to the first distribution locations on the first stand 22, and is lowered so that the flat surfaces 52 of die head 30 contacts with the slide that is positioned at this distribution locations. Die head 30 is positioned at an end place of the sample position location on the slide, and die head 30 is oriented to so that its end 44 is faced die head 30 with the direction that is moved. Die head 30 is with the pressure contact slide, and this pressure is the weight of distribution system 34 and by the combination of 74 applied pressures of spring. The amount of the contact that produces be distribution system 34 weight, spring 74 spring constant and be applied to the function of the decrement of spring 74. Usually, the contact that produces at about 10N to about the 35N.
When die head 30 during near the end of sample position location, piston rod 86 stops with respect to the movement of syringe 20, and when die head 30 arrives the end of sample position location, distribution system 34 moves up to promote die head 30, so that its disengaging contacts with slide, meanwhile, piston rod 86 is retracted a little with respect to syringe 20.
If the liquid sample in the syringe 20 will be used to form more than a film, so distribution system 34 is moved to the second slide on the stand 22, and if necessary, distribution system 34 is moved to follow-up slide on the stand 22 and duplicate allocation step. In typical experimental provision (set up), can form four films of as many as by each syringe 20.
In case formed described film, then just distribution system 34 is moved to syringe cap and die head removes platform 32, be similar to as previously described remove cap 36 from syringe 20, remove die head 30 from syringe 20 there.
Then distribution system 34 is moved to stand 28, and is placed on the first cap position, and with its reduction so that the end of syringe 20 engage with new cap 36. Then distribution system 34 is moved to the position for the receiving vessel of used syringe 20, and syringe 20 is released so that it falls into this vessel. Used syringe 20 can be dropped, if perhaps they contain still interested liquid preparation, so just it is collected for re-using. If the latter, receiving vessel can be controlled on environment so, for example by cooling.
For other syringe 20, repeat this order.
In case stand 22 has had the film that is formed on its whole slides, computer just can suspend to allow from framework 12 and removes this stand 22, and randomly, supplementary injection device stand 18 and die head stand 26 and cap stand 28, and the stand 22 that will newly load inserts in the framework 12. Then can be by foregoing processing slide, to form solid film.
According to the present invention, in selectable embodiment, each has the die head 30A (seeing Fig. 6 A to Fig. 6 C) of elongate body 40A, have in this embodiment round nose 42A, round nose 44A and be centrally located on annular protuberance 46A on its upper surface, annular protuberance 46A is coaxial with the cylinder hole 48A among the main body 40A. The upper end of annular protuberance 46A in the 47A place by reaming, with the port of export of auxiliary positioning syringe 20.
Be processed with or be molded with notch 54A among the lower flat surfaces 52A of the main body 40A of die head 30A, notch 54A is opened on the end 42A of main body 40A and from this end 42A to opposite end 44A along the total length longitudinal extension of die head 30A. The size of notch 54 will be shaped to the film that can produce required size as previously described.
To the present invention be described with further reference to the following example now.
Embodiment 1
With paint sample with have the adhesive sample (Ablebond 8200C, the epobond epoxyn of the filling silver that can obtain from Ablestik) of about 10Pa.s dynamic viscosity, prepare 10ml syringe 20 with about 5Pa.s viscosity.Use as with reference to the described die head 30 of Fig. 3 A to Fig. 3 C according to the present invention, on microslide, produce film with syringe.Notch in the die head 30 is that 17mm is long, 10mm is wide, and has the degree of depth of 75 μ m and 450 μ m respectively.The line of rabbet joint 50 of die head 30 that leads to notch is apart from the front end 10mm of die head 30, and wide be 1mm.Make paint films dry under environment temperature.Make binder film in baking oven in about 175 ℃ of curing.
Use micrometer to locate to measure film in three positions (position 1 of table, position 2 and position 3) that are arranged on the longitudinal axis of film then, position 2 is at approximate half the length place along the length of film, and position 1 and position 3 be 2 both sides in the position.
Use is had the paint sample film that the die head of the 75 μ m degree of depth makes be numbered 1 to 8, and use is had the paint sample film that the die head of the 450 μ m degree of depth makes be numbered 9 to 16, and the result who measures provides in table 1.Provided along the aging relative standard deviation (%RSD) of every group of % that measures of the length of film, and at every group of %RSD that measures of each measurement point.Similarly, the adhesive sample film is numbered 17 to 24 and 25 to 32 respectively, the result provides in table 2.
Embodiment 2 (comparative example)
On microslide, use the adhesive tape of approximate 130 μ m to form passage, employed liquid sample produces two groups of films among the use embodiment 1 on this microslide, first group of slide only has the individual layer adhesive tape along its every side, and second group of slide has three layers of adhesive tape along its every side.The liquid sample that is deposited on the slide uses scraping blade smooth.Press described in the embodiment 1, make the dry or curing of film, and press the thickness of the measurement film described in the embodiment 1.
To use individual layer adhesive tape thickness, promptly the paint sample film of making in the passage with approximate 130 μ m nominal depth is numbered 1C to 8C, and will use three layers of adhesive tape thickness, promptly the paint sample film of making in the passage with approximate 390 μ m nominal depth is numbered 9C to 16C, and the result provides in table 3.Similarly, the adhesive sample film is numbered 17C to 24C and 25C to 32C respectively, the result provides in table 4.
Table 1
| Sample | Position 1 | |
Position 3 | ％RSD |
| 1 | 26 | 28 | 29 | 5.52 |
| 2 | 33 | 32 | 33 | 1.77 |
| 3 | 29 | 31 | 31 | 3.81 |
| 4 | 34 | 32 | 27 | 11.63 |
| 5 | 30 | 32 | 33 | 4.82 |
| 6 | 32 | 34 | 34 | 3.46 |
| 7 | 30 | 28 | 25 | 9.10 |
| 8 | 31 | 33 | 31 | 3.65 |
| ％RSD | 8.19 | 7.11 | 10.44 | |
| 9 | 114 | 129 | 120 | 6.24 |
| 10 | 109 | 119 | 118 | 4.78 |
| 11 | 113 | 122 | 112 | 4.76 |
| 12 | 123 | 131 | 127 | 3.15 |
| 13 | 119 | 124 | 123 | 2.17 |
| 14 | 127 | 132 | 126 | 2.50 |
| 15 | 128 | 133 | 131 | 1.93 |
| 16 | 126 | 129 | 130 | 1.62 |
| ％RSD | 6.12 | 4.01 | 5.34 |
Table 2
| Sample | Position 1 | |
Position 3 | ％RSD |
| 17 | 45 | 46 | 50 | 5.63 |
| 18 | 51 | 44 | 44 | 8.72 |
| 19 | 49 | 49 | 49 | 0.00 |
| 20 | 48 | 42 | 41 | 8.67 |
| 21 | 46 | 46 | 40 | 7.87 |
| 22 | 48 | 48 | 48 | 0.00 |
| 23 | 45 | 45 | 44 | 1.29 |
| 24 | 48 | 43 | 43 | 6.46 |
| ％RSD | 4.36 | 5.26 | 8.29 | |
| 25 | 189 | 176 | 187 | 3.80 |
| 26 | 187 | 178 | 182 | 2.47 |
| 27 | 185 | 176 | 177 | 2.75 |
| 28 | 182 | 176 | 184 | 2.30 |
| 29 | 184 | 179 | 182 | 1.39 |
| 30 | 176 | 177 | 169 | 2.51 |
| 31 | 186 | 176 | 186 | 3.16 |
| 32 | 176 | 177 | 173 | 1.19 |
| ％RSD | 2.65 | 0.64 | 3.56 |
Table 3
| Sample | Position 1 | |
Position 3 | |
| 1C | ||||
| 56 | 57 | 65 | 8.31 | |
| 2C | 47 | 43 | 40 | 8.10 |
| 3C | 39 | 42 | 40 | 3.79 |
| 4C | 48 | 55 | 55 | 7.67 |
| 5C | 59 | 57 | 54 | 4.44 |
| |
50 | 50 | 59 | 9.80 |
| 7C | 61 | 55 | 57 | 5.30 |
| 8C | 82 | 69 | 81 | 9.35 |
| ％RSD | 26.42 | 17.79 | 26.09 | |
| 9C | 134 | 136 | 140 | 2.24 |
| 10C | 130 | 129 | 127 | 1.19 |
| 11C | 126 | 129 | 114 | 6.45 |
| 12C | 141 | 140 | 134 | 2.74 |
| 13C | 138 | 142 | 136 | 2.20 |
| 14C | 137 | 123 | 140 | 6.81 |
| 15C | 129 | 125 | 114 | 6.33 |
| 16C | 137 | 134 | 133 | 1.55 |
| ％RSD | 3.89 | 5.22 | 8.18 |
Table 4
| Sample | Position 1 | |
Position 3 | |
| 17C | ||||
| 62 | 61 | 57 | 4.41 | |
| 18C | 67 | 69 | 69 | 1.69 |
| 19C | 65 | 69 | 70 | 3.89 |
| 20C | 67 | 67 | 70 | 2.55 |
| |
60 | 58 | 61 | 2.56 |
| |
56 | 61 | 60 | 4.48 |
| |
56 | 59 | 61 | 4.29 |
| 24C | 59 | 60 | 63 | 3.43 |
| ％RSD | 7.32 | 7.25 | 7.96 | |
| 25C | 166 | 166 | 171 | 1.72 |
| 26C | 168 | 167 | 174 | 2.23 |
| 27C | 169 | 173 | 167 | 1.80 |
| 28C | 175 | 167 | 173 | 2.43 |
| 29C | 182 | 175 | 184 | 2.62 |
| 30C | 172 | 171 | 174 | 0.89 |
| 31C | 163 | 164 | 168 | 1.60 |
| 32C | 179 | 178 | 181 | 0.85 |
| ％RSD | 3.81 | 2.89 | 3.39 |
Can find out that from the comparison of the %RSD numerical value of the %RSD numerical value of each film and each measurement point on the film film that forms according to the present invention is comparable to the film that uses known technology to form at least.In addition, with the film that uses known technology to make relatively, the film formed repeatability (the %RSD numerical value of measurement point) of the film of making according to method of the present invention has improved, especially for thinner film with for more low viscous material.
Embodiment 3
Use method of the present invention on slide 102, to prepare adhesive multilayer complex films 100.Use as with reference to the described die head 30A of Fig. 6 A to Fig. 6 C, first rete 104 of first electroconductive binder is deposited on the slide 102, and die head 30A has 20mm long (place, summit at its round nose 42A and round nose 44A is measured), 10mm is wide and the dark notch of 220 μ m.Make first rete, 104 curing ovens then.
Use as with reference to the described second die head 30A of Fig. 6 A to Fig. 6 C, with second, second rete 106 of different electroconductive binder is deposited on first rete 104, die head 30A has 20mm long (place, summit at its round nose 42A and round nose 44A is measured), 10mm is wide and the dark notch of 500 μ m.Make second rete, 106 curing ovens then.
For making the composite membrane 100 can be detected, the composite membrane on the slide 102 100 is encapsulated in the epoxy resin 108, solidify then, and the composite membrane 100 sealed and slide 102 cut apart and polish.The MIcrosope image of the cross section of multilayer complex films 100 is shown in Fig. 7.In image, can clearly see the interface between two retes 104 and 106 of adhesive.The thickness of first rete 104 is about 145 μ m, and the thickness of second rete 106 is about 85 μ m.Generally, the thickness of multilayer complex films 100 is about 230 μ m.Use laser profile measuring instrument (laser profilometer) to study the profile (profile) of composite membrane 100, the thickness that has shown composite membrane 100 from the 3-D view of laser profile measuring instrument along its length and width very evenly and with the consistency of thickness that obtains from MIcrosope image.
Embodiment 4
For paint multilayer complex films 110 is described, use as with reference to the described die head 30A of Fig. 6 A to Fig. 6 C, first rete 114 of water-based emulsion lacquer is deposited on the slide 112, and die head 30A has 20mm long (place, summit at its round nose 42A and round nose 44A is measured), 10mm is wide and the dark notch of 220 μ m.Make first rete 114 dry under environmental condition then.
Use as with reference to the described second die head 30A of Fig. 6 A to Fig. 6 C, second rete 116 that just has the water-based paint of different colours is deposited on first rete 114, and die head 30A has 20mm long (place, summit at its round nose 42A and round nose 44A is measured), 10mm is wide and the dark notch of 500 μ m.Make second rete 116 dry under environmental condition then.
For making the composite membrane 110 can be detected, the composite membrane on the slide 112 110 is encapsulated in the epoxy resin 118, solidify then, and the composite membrane 110 sealed and slide 112 cut apart and polish.The MIcrosope image of the cross section of multilayer complex films 110 is shown in Fig. 8.In image, can clearly see the interface between two retes 114 and 116 of paint.The thickness of first rete 114 is about 47 μ m, and the thickness of second rete 116 is about 74 μ m.Generally, the thickness of multilayer complex films 110 is about 121 μ m.Use the laser profile measuring instrument to study the profile of composite membrane 110, the thickness that has shown composite membrane 110 from the 3-D view of laser profile measuring instrument along its length and width very evenly and with the consistency of thickness that obtains from MIcrosope image.
Should understand, the paint that uses different colours in this embodiment only is the formation of multilayer complex films for convenience of explanation, and use method and apparatus of the present invention can study other paint system, for example use the colored paint that paints such as priming paint, bottoming and finish paint and do not have colored paint.
Claims (31)
1. method that on substrate surface, forms film, described method comprises:
Provide and hold the container that place, the sample position location on described substrate surface is formed the liquid sample of film, described container has the outlet that comprises die head, described die head has tabular surface, described tabular surface can contact with described substrate, define the passage that is used for receiving at least a portion of described liquid sample with this from described container
Described die head is contacted with the end place of described substrate in described sample position location,
Make described liquid sample extrude and enter described passage by described die head, simultaneously, described die head and described substrate are moved each other in contact and relatively, described thus die head moves towards the far-end of described sample position location, with the film at the described liquid sample of place, described sample position location deposition.
2. method according to claim 1, wherein said container is a tube.
3. method according to claim 1 and 2, it comprises: to produce sucking fit betwixt described container is engaged by causing described container and described die head relatively moving between the two with described die head.
4. according to each described method in the aforementioned claim, it comprises: the described liquid sample in the described container is exerted pressure, so that described liquid sample flows through described die head.
5. according to each described method in the aforementioned claim, it comprises: the described liquid sample in the described container is exerted pressure, so that described liquid sample flow to the main volume that is enough to fill in the described die head.
6. according to each described method in the aforementioned claim, it comprises: form described passage by the notch that provides described liquid sample to flow in the tabular surface of described die head.
7. method according to claim 6, wherein said notch fully longitudinally extend through the opposite end of the tabular surface of described die head up to described die head, to form opening thus.
8. method according to claim 6, wherein said notch only part longitudinally extend through the tabular surface of described die head, extend to an end of described die head at least from the entrance that described liquid sample enters described notch, to form opening thus.
9. according to each described method in the aforementioned claim, wherein said liquid sample has in the about dynamic viscosity of 0.05Pa.s in about 100Pa.s scope.
10. according to each described method in the aforementioned claim, wherein said film comprises the composite membrane with at least two retes, by being deposited on first rete on the described surface and second rete being deposited on described first rete then, and if desired, follow-up rete is deposited on described second rete and the follow-up rete in turn, forms described composite membrane.
11., wherein be assigned to few two kinds of liquid samples in the punishment of described lip-deep sample position location according to each described method in the aforementioned claim.
12., wherein in single substrate, form membrane array according to each described method in the aforementioned claim.
13., wherein in single substrate, form each film in the membrane array according to each described method in the aforementioned claim.
14. according to each described method in the aforementioned claim, it comprises: abandon described die head later on forming at least one film with described die head.
15. each place, sample position location on substrate surface forms the method for a plurality of films, it comprises:
(a) provide multiple liquid sample in corresponding syringe, described syringe is at the corresponding cap closure of its port of export quilt;
(b) concurrently or preferred sequence ground, remove described cap and die head is coupled to the port of export of described syringe from each syringe, each described die head can contact with described substrate, defines the corresponding passage of at least a portion that is used for receiving liquid sample with this;
(c) concurrently or preferred sequence ground, corresponding described die head is contacted with the end place of described substrate in corresponding described sample position location;
(d) concurrently or preferred sequence ground, make the liquid sample in each corresponding syringe extrude and enter corresponding described passage by corresponding described die head, simultaneously, described die head and described substrate are moved each other in contact and relatively, described thus die head moves towards the far-end of described sample position location, with the film at the described liquid sample of place, described sample position location deposition.
16. be used on substrate surface, forming the equipment of film, it comprises substrate support device and distribution system, described distribution system is used in the operating period of described equipment at least a liquid sample being distributed in the place, lip-deep sample position location of the substrate of being supported by described substrate support device, described distribution system comprises the clamping device that is used for fixing container, in use, described container receiving fluids sample, described container has the outlet that comprises die head, described die head has tabular surface, described tabular surface can contact with described substrate, define the passage that is used for receiving at least a portion of described liquid sample with this from described container, described distribution system can be operated described die head is contacted with the end place of described substrate in described sample position location, simultaneously, described distribution system side by side can be operated basically described die head and described substrate are moved each other in contact and relatively, described thus die head moves towards the far-end of described sample position location, with the film at the described liquid sample of place, described sample position location deposition.
17. equipment according to claim 16, wherein said die head has the notch in its tabular surface.
18. according to claim 16 or 17 described equipment, wherein said notch fully longitudinally extends through the opposite end of the tabular surface of described die head up to described die head, to form opening thus.
19. according to claim 16 or 17 described equipment, wherein said notch only part longitudinally extends through the tabular surface of described die head, extends to an end of described die head at least from the entrance that described liquid sample enters described notch, to form opening thus.
20. according to each described equipment in the claim 16 to 19, wherein said distribution system comprises the device that the liquid sample in the described container is exerted pressure.
21. according to each described equipment in the claim 16 to 20, wherein said distribution system comprises the piston rod that can engage with the piston in the described container, described thus piston is removable to be realized the positive displacement of the described liquid sample in the described container or retreats.
22. equipment according to claim 21, wherein by be connected to described piston rod, by the stepping motor driven lead screw, described piston rod can move with respect to described clamping device.
23. according to claim 21 or 22 described equipment, wherein said piston rod can engage with described piston by second clamping device.
24. equipment according to claim 22, wherein said second clamping device comprises at least one spring steel clamping device that can move between non-moving position and moving position, more preferably be two spring steel clamping devices, in described moving position, described clamper engages described piston.
25. according to each described equipment in the claim 16 to 24, it comprises automation processing equipment, described automation is handled equipment and is used for index described substrate support device respect to one another and described distribution system, thus in use, can on the substrate surface at least two films be deposited on the place, sample position location that has living space each other on the described surface and concern.
26. a die head, it comprises main body and the liquid flow passageway with tabular surface, is formed with the notch that is used to receive liquid in described tabular surface, and described liquid flow passageway runs through described main body and ends at described notch.
27. equipment according to claim 26, wherein said notch fully longitudinally extend through the opposite end of the tabular surface of described die head up to described die head, to form opening thus.
28. die head according to claim 26, wherein said slot-open-section longitudinally extends through the described tabular surface of described die head, at least extend to an end of described die head from described path, to form opening thus, thus in use, the described end of described die head is a tail end with respect to the moving direction of described die head.
29. die head according to claim 23, wherein said half groove longitudinally extends beyond described path towards the front end of the described die head for the moving direction of the described die head in using.
30. according to each described die head in the claim 27 to 29, wherein said path ends at the line of rabbet joint of the whole width that extends described notch basically.
31. at least one membrane array more preferably is to comprise at least two membrane arrays and each described membrane array all in suprabasil film storehouse, wherein each film sample for reference position location is positioned evenly in the described array.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0618293A GB0618293D0 (en) | 2006-09-18 | 2006-09-18 | Film formation and evaluation |
| GB0618293.5 | 2006-09-18 | ||
| GB0714428.0 | 2007-07-24 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101522314A true CN101522314A (en) | 2009-09-02 |
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ID=37310076
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007800275816A Pending CN101522314A (en) | 2006-09-18 | 2007-09-18 | Film formation and evaluation |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN101522314A (en) |
| GB (1) | GB0618293D0 (en) |
-
2006
- 2006-09-18 GB GB0618293A patent/GB0618293D0/en not_active Ceased
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2007
- 2007-09-18 CN CNA2007800275816A patent/CN101522314A/en active Pending
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| Publication number | Publication date |
|---|---|
| GB0618293D0 (en) | 2006-10-25 |
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