CN1043614C - Method and apparatus for drying of polymer protective layer which has been applyed with solution on surface of articles - Google Patents

Method and apparatus for drying of polymer protective layer which has been applyed with solution on surface of articles Download PDF

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CN1043614C
CN1043614C CN92114839A CN92114839A CN1043614C CN 1043614 C CN1043614 C CN 1043614C CN 92114839 A CN92114839 A CN 92114839A CN 92114839 A CN92114839 A CN 92114839A CN 1043614 C CN1043614 C CN 1043614C
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coating
temperature
chamber
goods
polymer
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CN1086744A (en
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V·A·佩米切夫
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Nauchno-Proizvodstvennaya Aktsionernoe Obschestvo Zakrytogo Tipa "tekhnolo Firma
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Nauchno-Proizvodstvennaya Aktsionernoe Obschestvo Zakrytogo Tipa "tekhnolo Firma
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Abstract

The present invention provides a method and an apparatus for drying a polymer protective layer which is applied with solution on an article surface. The method comprises steps as follows: a coating layer is carried out the heat preservation for 20 seconds to 1 hours under room temperature. Under elevated temperature and sufficient high surplus pressure for suppressing the development of a micro crack, the coating layer is carried out the heat preservation within such a time. The coating layer is cooled to the room temperature. The apparatus comprises a high temperature room (13) connected with a high pressure pipeline (8). A charge opening (14) and a discharge opening (15) are respectively arranged, and a heater (24) is arranged. The present invention is applied when a microcircuit is produced and a thin polymer insulation layer is formed.

Description

To carrying out dry method and apparatus at the polymer protective layer of product surface coating by solution
The invention belongs to microelectronics and electrotechnics field, specifically, belong to and prepare with solution in the method for product surface coat polymers protective layer and implement the equipment of this method.
In the planar technique of semiconductor device and microcircuit; well-known drying solution is coated in the method for the polymer protective layer of product surface; be included in the step of this protective finish of insulation under the process chamber temperature, subsequently at the step and the cooling step that under the temperature that raises, are incubated under the pressure of surplus.In this case with regard to exist to obtain the flawless film of high-quality and during certain in keep the problem of its protective value.Microcrack and bubble can produce considerable influence to the rete protective value, and they are (so-called dry, we are interpreted as it by the process of deviating from solvent in the polymer film) takes place during along with drying physical chemical process and formation and development.
Coating material is carried out dry process comprise the solvent (liquid diffusion) that removes in the polymer itself, remove the solvent (gaseous diffusion) in the gas medium and make solvent become steam (phase transition of the first kind) by liquid state.The dynamics of said process has determined the mechanism that solvent removes from coating.
Dry initial period carries out under process chamber temperature (20~24 ℃), it is characterized in that the content height of solvent in the polymer coating and the speed that solvent liquid spreads thereof are fast.Along with coating is dried, the diffusion of solvent in polymeric material is slack-off, thereby dry speed is descended.
People know, by under the process chamber temperature polymer coating being carried out primary drying, can not obtain very high protective value value (adhesion, zero defect).
Thereby to be incubated at elevated temperatures in second stage.The basis that temperature is selected is must reach the high fluidity of polymer to increase diffusion velocity and to eliminate the coating internal stress, but also to consider the thermal stability of polymeric material, because high temperature and long effect thereof can cause undesirable thermal degradation or heat polymerization.
Initial period carries out the polymer coating insulation at elevated temperatures, can find that the speed that removes of solvent sharply increases.After reaching its maximum, this speed just drops to null value subsequently.
It has been generally acknowledged that, solvent evaporation appears on the outer surface of coating and in, also have phase transformation (evaporation), i.e. inner vapor formation effect on the gas microcrack surface that exists in the coating.
Experiment confirm inner vapor form and protective value between contact, for example photo resistance coating.The dynamics of microcrack internal solvent evaporation process is determined by series of factors: comprising the content of solvent in coating; The vapour pressure of solvent; The original shape of microcavity and size; The distribution density of microcrack in the coating volume; The liquid diffusion coefficient of solvent; The temperature of the viscosity of polymer coating and surface tension and coating.
Along with the quickening of inner vapor formation speed, defective increase and coating descend to the adhesion of goods.The generation of this situation is that it ruptures on the coating outer surface subsequently owing to being reached by the result of the saturated microcrack development of solvent vapour.
Be that the microcrack of sealing is with respect to residing position, interface between coating outer surface and coating and goods to what the defective forming process played an important role.For example, the microcrack of close coating outer surface breaks and does not damage the deep layer of polymer coating, also can not cause just like the influence that microcrack caused that is in goods and polymer coating boundary its protective value (adhesion).And the latter can also produce the broken hole that pierces through except making the disbonding when rupturing on the outer surface.Being arranged in the microcrack in the intermediate layer of polymer coating, is the precondition that causes the broken hole that pierces through, and as the place of this coating stress concentration, can weaken its adhesion to goods.
Inner vapor formation effect in the high protective finish of the first drying stage solvent can not play tangible effect for the protectiveness that reduces polymer coating.
This can be explained by following reason: the liquid diffusion coefficient height in the protective finish helps the evaporation of solvent; Polymer solution is in the high fluidity state, helps to strain the microcrack that is produced.
Along with the decline of solvent, polymer coating viscosity occurring increases, and lose the plane whole put ability (the whole ability of putting in so-called plane, we be interpreted as that polymer is set up flat surface and with the ability of the jagged edge tensioning of the microcrack opened).
Owing to lack suitable method, the flowability that determine solution is impossible for the accurate moment of the microcrack deficiency of the dangerous shape and size of tension.Can only think that for most photo resistance layer, it occurs in to removing after the centrifugal action that residue carried out on the polymer protective finish finishes from certain accuracy that real data is confirmed.
By the gas microcrack is produced reason and as the research that weakens the adhesion reason, should be understood that the size of these microcracks and the polydispersion characteristic of shape as the broken hole that pierces through in the protective finish.Certainly, along with the minimizing of large scale microcrack number, the protective value of this polymer coating will be improved greatly.
Meanwhile, even if there is undersized microcrack, the dry protective finish of crossing of long preservation also may be dangerous.
Probably each is required relevant process with executive condition and to protective value, determine the microcrack size of a permission, make protective value be unlikely and be reduced to below the essential value.
The most approaching with the present invention; be a kind of to carrying out dry method at the polymer protective layer of product surface coating by solution; may further comprise the steps: in the process chamber temperature range, this polymeric layer is incubated 20 seconds to 1 hour; then at elevated temperatures; the evolution that is enough to contain microcrack in the protective finish with the overpressure of improving its protective value under; dry polymer coating again; and the step that makes the cooling of this polymer coating is [referring to the 5th (53) phase of " electronic technology " magazine; 1975, B. П. Л ABP И IUeB,B.A. П EpeMbI Ш eBArticle " by removing the solvent Study on Mechanism in the photoresistance film ", P.58~65.]
The external pressure of surplus is to hinder that inner vapor forms and the factor of containment gas microcrack development when under the temperature conditions that raises protective finish being carried out drying.
Adopt the dry polymer coating of crossing of said method, have the broken edge of piercing through and the defective of weakness zone.Show therefrom and lose adhesion, thus the suitable time limit of shortening polymer coating.More than two shortcomings be that microcrack evolution when carrying out drying by polymer coating causes.
Under the temperature that improves,, can not guarantee to finish specification requirement to polymer coating protective value aspect in the evolution of polymer coating holding stage containment microcrack.
Existing realization is to the equipment by solution coat polymers protective layer drying means on goods, comprise the elevated-temperature seal chamber that at elevated temperatures polymer coating is incubated usefulness, this elevated-temperature seal chamber links to each other with pressure duct and is connected in the unlimited outlet of leading to space outerpace by the conduit of being with valve; This elevated-temperature seal chamber be equipped with charging door, the band sealing damper of band sealing damper discharge port, from charging door to discharge port transport the mechanism of goods and heater [referring to " electronics industry ", No.5 (77), 1979, Moscow, B.B.A AHY Ф P И eH К O,B. И .O CH И H, B.A. П EpeMbI Щ eB,B. Л .C AH Л epoB, B.H. Ц ApeB" form the complete set of equipments A Ф Ф-2 that the photoelectricity resistance layer is used ", P.50~52].
In this equipment, be incubated at elevated temperatures and set up superfluous pressure in the polymer coating step.In this case, have only pack into hot room and close the pressure that just might in hot room, set up surplus after the charging door by sealing damper of goods; And remove this overpressure, then must be cooled to and can eliminate the temperature that makes the microcrack evolution that protective value degenerates under the condition of normal pressure at polymer coating.
With respect to coating heating, even little hysteresis overpressure effect also can cause by the coating of the thickness of very little mark micron and the explicitly negative interaction that the coating thermal capacitance is brought.After coating was sent into the heating space of hot room, in fact this coating was heated to the temperature of high temperature indoor gas immediately; Yet can not set up superfluous pressure in moment.Before opening hot room taking-up goods, removed the moment of overpressure; this coating still is in similar heated condition; and under no overpressure, polymer coating is heated; will cause intensifying of inner vapor formation effect, thereby provide advantage for the development of microcrack in the protective finish.
As the task that basis of the present invention proposed, be to set up a kind of drying means that the polymer protective layer that is applied at product surface by solution is carried out, wherein the dry coating step will be set up a kind of like this drying condition under the process chamber temperature, promptly before improving temperature anticipation with the pressure of surplus; And set up a kind of like this condition at cooling step, promptly before interrupting the overpressure effect, reduce temperature earlier; Will found the equipment of this method of realization simultaneously, it need not big cost during fabrication, and convenient desirable.
Being proposed of task is to solve like this.To being undertaken may further comprise the steps in the dry method: in the process chamber temperature range, polymer protective layer is incubated 20 seconds to 1 hour by the polymer protective layer of solution in product surface coating; subsequently under the temperature that raises; can make under the overpressure of the microcrack evolution that its protective value degenerates and be incubated polymer protective layer being enough to containment, and the step that makes its cooling.According to the present invention; be enough to the needed overpressure of microcrack evolution that containment can make the protective value of protective layer degenerate; be in the process chamber temperature range insulation polymeric layer step in set up; and in cooling step, keep, up to reaching under atmospheric pressure conditions the temperature that can elimination can make the microcrack evolution that its protective value degenerates always.
This task solves simultaneously like this.In the equipment of this method of enforcement, comprise the elevated-temperature seal chamber that at elevated temperatures polymeric layer is incubated usefulness, this elevated-temperature seal chamber links to each other with pressure duct and is connected in the unlimited outlet of leading to space outerpace by the conduit of being with valve; This elevated-temperature seal chamber be equipped with charging door, the band sealing damper of band sealing damper discharge port, transport the mechanism and the heater of goods to discharge port from charging door.According to the present invention, the flow process along goods move was provided with an additional seal chamber in addition before hot room, made polymer coating dry under the process chamber temperature.It communicates with hot room by the charging door of the band sealing damper of hot room, and the charging door of the band sealing damper of oneself is housed, this chamber links to each other with pressure duct and the conduit by the band valve is connected in the unlimited outlet of leading to space outerpace, and be equipped with goods thus the charging door of additional seal chamber be transported to the mechanism of hot room charging door; And the flow process of moving along goods of the present invention, the additional seal chamber that a cooling polymer coating is used is set after hot room in addition, it communicates with hot room by the discharge port of band sealing damper, and the discharge port of the band sealing damper of oneself is housed, this mouthful links to each other with pressure duct and is connected in the unlimited outlet of leading to space outerpace by the conduit of being with valve, and the mechanism that goods is transported to the cooling chamber discharging opening by the discharging opening of hot room is housed.
In order to shorten cooling time, be preferably polymer coating coolant seal chamber and be equipped with cooling device in addition.
To being undertaken in the dry method by the polymer coating of solution in product surface coating; owing to set up superfluous external pressure in the step that coating is incubated under the process chamber temperature, reached this overpressure (can make the microcrack growth interruption that can cause the coating protection performance depreciation under this pressure) produces heat effect before to polymer coating possibility so just eliminated.
In addition; in the cooling step of polymer coating, set up overpressure; just may get rid of under atmospheric pressure and in the protective layer of heating, to discharge remaining solvent consumingly, and it is can cause producing on the polymer-coated surface making microcrack that its protective value reduces.
Subsequently will be by to the narration of specific embodiment and utilize description of drawings the present invention, wherein,
Fig. 1 represents that temperature T and pressure P (axis of ordinates) are for the relation curve of τ drying time (axis of abscissas) according to the polymer protective layer that is applied at product surface by solution is carried out dry method;
Fig. 2 represents the relation curve of solvent removal speed V (axis of ordinates) for τ drying time (axis of abscissas).
Fig. 3 is to carrying out desiccant equipment vertical section by solution at product surface coat polymers protective layer according to of the present invention.
May further comprise the steps carrying out dry method at product surface coat polymers protective layer by solution: under the process chamber temperature in 20 seconds to 1 hour the step I (Fig. 1) of heat insulation coating, during this period of time set up the external pressure of the surplus that can containment can make the microcrack development that the coating protection performance reduces in the heat preservation zone; The step II is at elevated temperatures, make the coating insulation under the external pressure of the surplus of the microcrack development that the coating protection performance is reduced, during this period of time be enough to the mechanical performance and the protective value that reach given, but be unlikely the structural change that causes after this coating is heated; The step III is for making coating be cooled to be in still not take place under the atmospheric pressure temperature that can make the microcrack development that the coating protection performance reduces under the external pressure of suitable surplus.
The step I is for example used centrifugation method from polymer solution is coated on the product surface with coating form.The rotation of the goods of band coating should be regarded as the incipient stage I of heat insulation coating step I under the process chamber fixed temperature ' (Fig. 1).In this case, can find the rate of drying maximum in the I ' stage that is in (Fig. 2), what at this moment take place is to cause by centrifugal action to force solvent to quicken diffusion with gaseous state.
The characteristics of this step I are that the content of solvent in the coating reduces, thereby its viscosity increases, and reduce the ability of the microcrack that is produced in the polymeric material tension coating simultaneously.Polymer coating carries out the transition to this state in the step I; guarantee that by during this period of time (I among Fig. 1 " stage) set up superfluous external pressure (this pressure can be contained inner vapor formation effect, thereby containment can make the development of the microcrack that the coating protection performance reduces) and prevent because the pore size that inner vapor formation effect causes increases.
In the process chamber temperature T IDown polymer coating is incubated to begin the stage I set up before the superfluous external pressure ' length, by reaching the required time decision of coating optimum state.For various concrete conditions, the sort of to be subjected to the microcrack influence on development less, and just the protective value minimum coating state that descends will be understood that it is best.This state is to be determined by the series of physicochemical of coating and mechanical property.At first be the thickness of coating, the content of solvent, its vapour pressure, the diffusion velocity of solvent, the viscosity of coating material, surface tension, gas porosity characteristic, temperature and the external pressure of coating.
Be perfectly clear, various types of polymer coatings all have optimum state of oneself and the insulation duration under the process chamber temperature.Time τ IDetermine by experimental technique, and for most polymer coatings, in the scope in 20 seconds to 1 hour.The temperature retention time τ of polymer coating in the step I for example IBe less than 20 and move clock, then remaining solvent will be very remarkable, thereby cause needing to add its eliminating of good general in the next step II.The temperature retention time of polymer coating in the step I surpasses one hour, can cause excessive increase but not improve its protective value drying time.
The characteristic of polymer and solvent, the temperature T of coating IIAnd to the requirement of its protective value, be to set up the suitably decisive factor of the superfluous external pressure of size, require this pressure basically in 0.3~0.8 MPa scope.Overpressure is lower than 0.3 MPa, is not enough for reducing the microcrack development.Overpressure is increased to is higher than 0.8 MPa, be helpless to improve the protective value of coating.
Step II (Fig. 1,2) is the temperature T that is raising II(Fig. 1), at the overpressure P that can contain the microcrack development ICarry out the coating insulation under the condition.
When temperature is elevated to T IIValue helps to reduce the viscosity of polymer coating, thereby causes the increase (II ' section among Fig. 2) of solvent removal speed V.At T IIMake the duration τ of polymer coating insulation under the temperature (Fig. 1) IIIBe 30 seconds to 1 hour, it depends on the thickness and the type of polymer coating, depends on the Products Quality and the specific heat that scribble this coating, depends on caloic transmittance process dynamics, depends on the thermal stability of coating temperature and polymer.
In the step II polymer coating insulation being less than for 30 seconds, is not enough to remove solvent from coating; And at elevated temperatures the polymer coating insulation is surpassed 1 hour, will cause this polymer coating structural damage, thereby cause that its protective value sharply descends.Therefore, for the elevated temperature T in the step II IIWith duration τ IIISelection, depend on the form of polymer coating.
For example for diazonium quinone photoresist (Ф OTopea И cTopHoe) coating, temperature T in the step II IIIn 80~100 ℃ of scopes, think working temperature.The temperature T of in the step II, using IIBe lower than 80 ℃, can not guarantee to remove fully solvent, thereby reduce the adhesion of coating product surface.Be higher than under 100 ℃ the temperature the polymer coating insulation, will be with the acceleration thermal degradation of polymer, thus influence the steady quality of protective value.
To based on the electronics of polymethyl methacrylate (a against corrosion Л e к TpoHope З И cT И BHoe) copolymer coated, one time of the temperature state of its drying steps II has roughly the same relation.Concerning it, at temperature range T IIWhen being 160~200 ℃, insulation duration τ IIIIt is 60 seconds to 1 hour.
Subsequent polymer coating is cooled to temperature T III(step III among Fig. 1), T IIIEqual T IThe speed that the removes V of solvent (step III among Fig. 2) in the step III will drop to zero gradually.
The equipment of enforcement to being used by the method for solution coat polymers protective layer drying on product surface comprises being used for the closed chamber 1 that under the process chamber temperature goods (not shown) that scribbles polymer coating is incubated that it is in first of the goods movement travel.This closed chamber 1 is equipped with the charging door 2 of band sealing damper 3 and the discharge port 4 of band sealing damper 5.Be equipped with in the closed chamber 1 and place platform 6 that goods use and the connecting gear 7 that goods is transported to discharge port 4 usefulness from charging door 2.Connecting gear 7 is in the present embodiment made the form of conveyer belt.
Closed chamber 1, process are equipped with the pipe joint 9 that is contained on closed chamber 1 shell wall of the additional conduits of pressure regulating valve 10,11 to connect with pressure duct 8.With the exception of this, the valve that can allow closed chamber 1 connect atmosphere also is housed on this conduit.
According to the movement travel of goods, after closed chamber 1 the elevated-temperature seal chamber 13 that at elevated temperatures polymer coating is incubated usefulness.
In the present embodiment, the discharge port 4 of closed chamber 1 is exactly the charging door 14 of hot room 13.Its discharge port 4 of 1 process of closed chamber communicates with hot room 13.
In addition, hot room 13 also is equipped with the discharge port 15 that sheds the band sealing damper 16 that goods use.Be equipped with in the hot room 13 and place platform 17 that goods use and goods are transported to the connecting gear 18 of discharge port 15 usefulness from charging door 14, it makes the conveyer belt form in the present embodiment.Closed chamber 13 links to each other with pressure duct 8 through being equipped with pipe joint 20 and pressure regulating valve 21,22,23.Heater 24 is housed in the hot room 13.According to the movement travel of goods, following is the additional seal chamber 25 of coating cooling after making polymerization after hot room 13.
Additional seal chamber 25 is equipped with the charging door 26 of band sealing damper 27, and it is again the discharge port 15 of hot room 13 simultaneously.This mouth 26 of 13 processes of hot room communicates with additional seal chamber 25.In addition, additional chamber 25 also is equipped with the discharge port 28 of band sealing damper 29.Be equipped with in the additional chamber 25 and place platform 30 that goods use and the connecting gear 31 that goods is transported to discharge port 28 usefulness from charging door 26.
Additional chamber 25 is through being equipped with the tube connector 32 of pipe joint 33 and pressure regulating valve 34~36 to link to each other with pressure duct 8.Below platform 30, be fixed with cooling device 37.
Be shown in solid arrow among Fig. 3 that gas is along the direction of catheter movement when setting up overpressure in closed chamber 1,13 and 25, the arrow of band dotted line is then represented by gas in the pipe is entered the direction that atmosphere deducts this pressure.
Distance between the article conveyor structure 18 in article conveyor structure 7 and the hot room 13 in the closed chamber 1 will be chosen in the length that is freely transmitted goods when being not less than sealing damper 5 and mouthfuls 4 and opening by chamber 1 to chamber 13.And the distance between article conveyor structure 18 and 31 is also kept same relation.
Realize the equipment of drying means of the present invention, carry out work in the following manner.
To be ready to the work of hot room 13 in advance.Need to shut sealing damper 5 and 16 for this reason, connect heater 24, open the valve 21 and 22 (valve 23 that is connected hot room 13 and atmosphere is all closed in whole arid cycle at polymer coating) of pressure duct 8.
, by connecting gear 7 goods that scribble polymer coating liquid on its surface are put on the platform 6 that is contained in the closed chamber 1 through the charging door 2 got through.Close the flashboard 3 of charging door 2 and open pressure regulating valve 10 and 11 (at this moment the valve 12 that is connected closed chamber 1 and atmosphere closes), in closed chamber 1, to set up superfluous pressure.Then the flashboard 5 of discharge port 4 is opened, and goods are delivered on the platform 17 in the hot room 13 by connecting gear 7 and 18.At this moment the pressure after raising in closed chamber 1 and the hot room 13 is the same.
In hot room 13 to the cooling chamber 25 that will be prepared in advance between the goods soak.To close the sealing damper 29 of discharge port 28 for this reason, close the valve 36 that is communicated with cooling chamber 25 and atmosphere, open the valve 34,35 of pressure duct 8 and connect cooling device 37.
In hot room 13 to scribbling goods when insulation of polymer protective layer on it, by open valve 11 and 12 and valve-off 10 removes after the overpressure in the chamber 1, the flashboard 3 that can open charging door 2 is with reception next group goods.
Coating in hot room 13 through the insulation of one period regular time after, open the flashboard 16 of discharge port 15, connect connecting gear 18 and 31 and goods are delivered on the platform 30 in the chamber 25, and close flashboard 27.After polymer coating is cooled to given temperature, open valve 36 to remove superfluous pressure, open the flashboard 29 of discharge port 28, connect article conveyor structure 31 and from chamber 25, draw off part.
In order to shorten the cooling time in additional seal chamber 25, can consider to adopt cooling device 37, aggravate coating cooling procedure in the chamber 25 by it.
Implement the equipment of the inventive method, can in the uninterrupted flowing water operation of goods, realize drying polymer protective layer.Just because of like this; for dissimilar protective finish; ratio between low temperature temperature retention time, high-temperature holding time and cooling time is different; this equipment can be in the chamber 1; several platforms 6,17 and 30 (not shown)s are arranged with the placement goods in 13 and 25, and connecting gear 7; 18 and 31 can be between the complementary platform in chamber 1,13 and 25 the dislocation goods.A kind of like this technical solution, might make this equipment with fixing cycling under continuous state.
In order more to be expressly understood essence of the present invention, below provide its specific embodiment.Embodiment
Below to comparing evaluation by the dry polymer coating of crossing of the inventive method and by the protective value of the dry coating of crossing of existing method.
For the photoresist polymer coating is carried out drying, once utilize existing equipment and according to equipment of the present invention.
The goods of packing in the closed chamber (Fig. 3) 1 of equipment of the present invention were once selected the glass plate of chromium plating as these goods, and scribbling thickness on it is the polymer protective layer of the diazonium quinone photoresist solution of 0.7 μ.After the photoresist layer drying, these goods are used as the blank of making optical mode.In the space of closed chamber 1, after its hermetically closing, by setting up the overpressure of 0.5 MPa by pressure duct 8 air feed, follow constant when it is incubated coating in each chamber 13 and 25 subsequently.Temperature retention time to protective layer in chamber 1 is 3 minutes, and temperature is 22 ± 2 ℃ in the chamber 1.Temperature retention time in chamber 13 is 15 minutes, and temperature is 100 ℃.Be 3 minutes the cooling time in the step III in chamber 25, is cooled to 22 ± 2 ℃ of end temperatures.
Check reaching as stated above, undertaken by universal method by the dry protective layer defective of crossing of known method.Result of the test is quoted in following table.
The index of these protection parameters is to determine according to the arithmetic mean for 10 tested goods.Evaluation for the qualified growth of coating; can be according to known protection parameter and standard; relatively with known method dry that cross and with the present invention dry protective finish through 2 and 4 months test index, and evaluate according to the goods number that does not satisfy this standard.
The protective value title of polymer coating The required standard of protective value Carry out the time protection parameter index relevant with test with drying means
The dry same day Through 2 months Through four months
According to the inventive method Adopt known method According to the inventive method Adopt known method According to the inventive method Adopt known method
1 3 4 5 6 7 8
Size is not more than the defective gross density (cm of 1 μ -2) Be not more than 0.20 0.03 0.09 0.028 0.16 0.04 0.29
Density (the cm of the wherein perverse broken hole of wearing -2) Be not more than 0.20 0.017 0.069 0.015 0.14 0.02 0.27
Density (the cm of residual chromium -2) Be not more than 0.20 0.013 0.021 0.013 0.02 0.02 0.02
The goods number of discontented foot protection performance standard 0 0 0 1 0 9
Cover layer is to the corrosion (μ) of protective finish Be not more than 0.2 0.1 0.15 0.1 0.2 0.12 0.35
Do not satisfy the goods number of above-mentioned standard 0 0 0 3 0 10
Cover layer greater than 0.5 μ corrodes (cm to the molten layer of polymer -1) Do not allow 0 0 0 0 0 0.01
Do not satisfy the goods number of above-mentioned standard 0 0 0 0 0 7

Claims (3)

1. the method for the polymer protective layer that forms of drying solution coated articles surface is included in the process chamber temperature range step that polymer protective layer is incubated 20 seconds to 1 hour; Subsequently under the temperature that raises, can make the step of this polymer protective layer of insulation under the overpressure of the microcrack evolution that its protective value degenerates being enough to containment; And the step that makes its cooling; it is characterized in that: be enough to the needed overpressure of microcrack evolution that containment can make the protective value of protective layer degenerate; be in the process chamber temperature range insulation polymer coating step in set up; and in cooling step, keep, reach under atmospheric pressure the temperature that can elimination can make the microcrack evolution that its protective value degenerates up to coating. always
2. equipment of implementing the described method of claim 1, comprise the elevated-temperature seal chamber (13) that at elevated temperatures polymer coating is incubated usefulness, this elevated-temperature seal chamber (13) links to each other with pressure duct (8) and passes through band valve (21,22,23) conduit (9) is connected in the unlimited outlet of leading to space outerpace, the charging door (14) of band sealing damper (5) is equipped with in this elevated-temperature seal chamber (13), the discharge port (15) of band sealing damper (16), transport mechanism (18) and the heater (24) that goods are used from charging door (14) to discharge port (15), it is characterized in that: the flow process of moving along goods, be provided with one before at hot room (13) and under the process chamber temperature, make the desiccant additional seal of polymer coating chamber (1), it communicates with hot room (13) by the charging door (14) of band sealing damper (5), and the charging door (2) of the band sealing damper (3) of oneself is housed, it links to each other with pressure duct (8) and passes through valve (10,11,12) conduit is connected in the unlimited outlet of leading to space outerpace, and be equipped with goods thus the charging door of additional seal chamber (2) be transported to the mechanism (7) of hot room (13) charging door (14); And the flow process of moving along goods, at hot room (13) the additional seal chamber (25) that a cooling polymer coating is used is set afterwards, it communicates with hot room (13) by the discharge port (15) of band sealing damper (16), and the discharge port (28) of the band sealing damper (29) of oneself is housed, it links to each other with pressure duct (8) and passes through band valve (34,35,36) conduit is connected in the unlimited outlet of leading to space outerpace, and the mechanism (28) that goods is transported to the cooling chamber discharging opening by the discharging opening (15) of hot room (13) is housed.
3. equipment according to claim 2 is characterized in that, the closed chamber that the cooling polymer coating is used (25) is equipped with cooling device (37) in addition.
CN92114839A 1992-11-07 1992-11-07 Method and apparatus for drying of polymer protective layer which has been applyed with solution on surface of articles Expired - Fee Related CN1043614C (en)

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SU444040A1 (en) * 1971-12-24 1974-09-25 Ордена Ленина Завод "Ленинская Кузница" The method of drying paint polymer coatings
DE2433310A1 (en) * 1974-07-11 1976-01-22 Georg Buechner Coating and baking enamel covered workpieces - has hot gas drying and baking system utilising spent hot gases to preheat drying air flow

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Publication number Priority date Publication date Assignee Title
SU444040A1 (en) * 1971-12-24 1974-09-25 Ордена Ленина Завод "Ленинская Кузница" The method of drying paint polymer coatings
DE2433310A1 (en) * 1974-07-11 1976-01-22 Georg Buechner Coating and baking enamel covered workpieces - has hot gas drying and baking system utilising spent hot gases to preheat drying air flow

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