CN110114668A - Alumilite process containing pigment handles plasma indicator - Google Patents

Alumilite process containing pigment handles plasma indicator Download PDF

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Publication number
CN110114668A
CN110114668A CN201780080935.7A CN201780080935A CN110114668A CN 110114668 A CN110114668 A CN 110114668A CN 201780080935 A CN201780080935 A CN 201780080935A CN 110114668 A CN110114668 A CN 110114668A
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pigment
plasma
indicator
red
alumilite process
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伊藤淳
浦谷昭太
作村武志
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Sakura Color Products Corp
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Sakura Color Products Corp
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/3065—Plasma etching; Reactive-ion etching

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Abstract

Problem of the present invention is that avoiding the pollution from the indoor composition for ink of chamber.As solution, the present invention provide it is a kind of make the hole formed by anodized contain made of pigment containing pigment alumilite process processing plasma indicator.

Description

Alumilite process containing pigment handles plasma indicator
Technical field
The present invention relates to a kind of plasma indicators.
Background technique
Various equipment, utensil used in hospital, research institute etc. etc., implements sterilization treatment to sterilize and sterilize. As sterilization treatment a kind of, it has been known that there is plasma sterilization processing.
Specifically, plasma sterilization processing is to generate plasma under the gaseous environment for generating plasma, by low The processing that wet bulk plasmon sterilizes to various equipment, utensil etc., so that it may be for low temperature sterilization processing this point It is advantageous.
In addition, corona treatment is applied not only to sterilization treatment, the plasma being also used in the manufacturing process of semiconductor element The plasma clean on the surface of the treated objects such as dry-etching and electronic component.
Plasma dry etch, it is however generally that, apply to the indoor electrode of reaction chamber being configured at as vacuum tank high Frequency power, to imported into reaction chamber it is indoor generate plasma gas carry out it is plasmarized and to semiconductor crystal wafer into The high-precision etching of row.In addition, plasma clean, it is precipitated on the surface by treated objects such as removal electronic components or attached Metal oxide, organic matter, burr etc., improve the wetability of zygosity or solder to improve adhesive strength, or improve With the adhesion or wetability of sealing resin.
Method as the terminal for detecting these corona treatments, it is known to as recorded in Patent Document 1, it will contain There is the composition for ink of pigment, specific surfactant, nonionic class surfactant to be coated on substrate, is placed on Method in reaction chamber etc..
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2015-013982 bulletin
Summary of the invention
Above-mentioned method, can it is simple, be detected positively in the indoor plasma of reaction chamber for carrying out corona treatment The irradiation of body, so that it may which the progress of plasma processing is by visual observation excellent for confirming.
However, in the chamber for carrying out corona treatment, if there is there is the film formed by composition for ink, due to plasma Body treatment conditions etc., pigment, surfactant and optionally vehicle also receives corona treatment cannot deny a part A possibility that gasifying.
Since a part gasifies, it is possible to generate polluter in the chamber for carrying out corona treatment, therefore according to being located The article of reason, it is necessary to avoid the pollution based on these polluters.
Present inventor has made intensive studies in order to solve the above problems, as a result, it has been found that by be made specific structure etc. Gas ions indicator can solve the above subject, so as to complete the present invention.
It is described in detail below.
1. a kind of alumilite process containing pigment handles plasma indicator, which is characterized in that make by anodic oxidation Reason and the hole formed contain pigment and form.
2. alumilite process according to 1 containing pigment handles plasma indicator, which is characterized in that pigment be selected from Anthraquinone pigments, methine class pigment, azo pigment, phthalocyanines pigment, triphenylmethane pigment, edible pigment and xanthene class It is at least one kind of in pigment.
3. the alumilite process according to 1 or 2 containing pigment handles plasma indicator, which is characterized in that the hole It is formed through sealing pores.
According to the present invention, in the chamber for carrying out corona treatment, by being placed under plasma environment, certainly It can make indicator discoloration, colour killing, therefore can correctly indicate the implementation of corona treatment.
At this point, the discoloration of indicator, achromatic condition can be adjusted according to the size of hole or the degree of sealing pores.
Further, since there is no the ingredient other than the pigments such as surfactant, especially organic compound, and in substrate surface It is upper that pigment is not present, but be present in hole, so ingredient other than pigment etc. will not occur in corona treatment Gasification, the probability that the object of the corona treatment caused by can more reducing thus pollutes.
Detailed description of the invention
Fig. 1 is the schematic diagram of the process in the hole for make aluminium formed body surface containing pigment.
Symbol description
1- aluminium formed body；2- anodized film；3- hole；4- pigment.
Specific embodiment
Plasma indicator of the invention can be pre-formed hole by carrying out alumilite process processing to aluminum substrate Then gap is obtained next, the hole is made to contain pigment and implementing or not implementing sealing pores.
Hereinafter, being illustrated to the manufacturing method of plasma indicator of the invention.
[alumilite process of substrate is handled]
Substrate used in the present invention is generally also possible to referred to as aluminium conjunction although can be the material being only made of aluminium The material (for example, Al-Mn class alloy, Al-Mg class alloy, Al-Mg-Si class alloy etc.) of gold, as long as at by anodic oxidation Manage and formed the material of hole.Furthermore it is metallic alloying with others to be also possible to aluminum material itself, and is coloured Material.Hereinafter referred to as aluminium formed body.
The shape of substrate can be plate, rodlike, linear, foil-like etc., can also be with other materials (metal, plastics, sticker Deng) form composite material.For example, plate or foil-like substrate the back side via resin film layer formed adhesive phase material It can.At this point, when in use, indicator can be fixed on arbitrary position.Furthermore aluminium formed body can also be by grinding, erosion The pre-treatments such as quarter, delustring (mat finish) and the processing of bright face.
Before anodized, by aluminium formed body by well known method, such as it is impregnated in one timing of sodium hydrate aqueous solution Between, degreasing is carried out by washing.
Alumilite process processing generally in order to assign aluminium formed body surface (aluminum material) corrosion resistance and dicoration and into Capable processing is identical, needs for that can form the processing of hole on anodized film.
It carries out the anode of aluminium formed body and anodic oxidation treatment device in electrical contact, is impregnated in electricity together with the anode and cathode It solves in liquid, forms anodized film by being powered on above-mentioned aluminium formed body between above-mentioned anode and cathode.It is powered simultaneously It is not limited to direct current, other known methods such as electric current of alternating current or impulse waveform can also.
As used electrolyte at this time, it is preferable to use containing at least any one in sulfuric acid, maleic acid, malonic acid, oxalic acid The solution of 3~30 weight % of the electrolyte of kind.Although being not particularly limited to this, in the silver color of the color that reflects aluminium In the case of preferably sulfuric acid, preferred oxalic acid in the case where gold.Furthermore 0~40 DEG C is set by electrolysis temperature, current density is 0.5~3.0A/dm2, implement 5 points~1 hour anodized.
In addition, adding metal ion in the electrolytic solution at this point, passing through, available is not the silver color for reflecting the color of aluminium, But the alumilite process of coloring handles surface.Such as addition copper ion obtains the aluminium anode oxide film for being colored as green.
The hole of generation, such as shown in Fig. 1 (a), be formed as at the anodic oxidation that the surface of aluminium formed body 1 is formed Manage the hole 3 in the space of the long column shape of the depth direction extension of film 2.But relative to aluminium formed body surface, it is not limited in shape At right angle as shown in the figure, it is effectively shown as the irregular shape such as bending, branch.Although the aperture of its opening portion can root The hole for the anodized film for arbitrarily adjusting according to anodized condition, but being generated in the present invention according to the process Gap, the aperture of opening portion are 5~300nm, preferably 5nm~50nm, more preferably 8~50nm.It is then difficult to if more than 300nm Anodized film is set to become uniform film, and the perforated membrane less than 5nm is then not easy to obtain.
In addition, the length of hole 3 is not particularly limited, as long as the pigment measured required for coloring can be adequately put into hole Required length in gap, therefore, for from aluminium surface to 2~50 μm of thickness direction of length, preferably 3~40 μm, into One step is preferably 3~20 μm.
After the processing of coloring alumilite process or the alumilite process processing of non-coloring, to be further formed coloring Implementing re-electrolysis processing for the purpose of film can also.Re-electrolysis processing will be impregnated by the aluminium formed body of alumilite process processing Electrolysis processing is carried out in the aqueous solution containing metal ion.For example, can be using the water-soluble of the ion containing nickel, silver, copper etc. Liquid is coloured with the color of the metal restored from these ions.
It is handled by re-electrolysis, is sent out in the bottom surface for the hole 3 that the alumilite process surface of coloring or non-coloring is formed to inner face The precipitation of raw metal, forms the coloring film from metal.
Re-electrolysis processing, by being dipped through the aluminium of alumilite process processing in the electrobath containing metal ion, by this Alumilite process process film is as electrode, then impregnates other electrode, these electrodes are passed through with the electricity of alternating current or impulse waveform Stream etc. and implement.
It, can be from process as the alumilite process substrate before setting pigment in the present invention by arbitrarily implementing these processing It is selected in coloring alumilite process or the aluminium of non-coloring alumilite process processing, it is also an option that the presence or absence of re-electrolysis processing, Therefore it can be selected and applied from total 4 kinds of alumilite process processing substrate.
By implementing coloring alumilite process processing, and/or implementation re-electrolysis processing, aluminum substrate after treatment can be made The color on surface become the silver color for not reflecting the color of aluminium, green yellow or red etc. other colors.As a result for The color of pigment more easily can confirm corona treatment by visual observation.
[pigment]
Pigment used in the present invention needs for that can dye to anodizing of aluminium process film, and by etc. from The substance of daughter irradiation meeting colour killing or discoloration.As above-mentioned pigment, using selected from anthraquinone pigments, methine class pigment, azo It is class pigment, phthalocyanines pigment, triphenylmethane pigment, xanthene class pigment, at least one kind of in edible pigment.
As long as anthraquinone pigments are using anthraquinone as the substance of basic framework, there is no limit, and well known Anthraquinones can be used Disperse dyes etc..Wherein, particularly preferably with the anthraquinone pigments of amino.More preferably have in primary amino group and secondary amino group extremely The anthraquinone pigments of few a kind of amino.At this point it is possible to 2 or more various amino, these amino mutually can it is identical or It is different.
More specifically, such as Isosorbide-5-Nitrae-diamino-anthraquinone (C.I.Disperse Violet 1), 1- amino-4-hydroxy-can be enumerated 2- methylamino anthraquinone (C.I.Disperse Red 4), 1- amino -4- methylamino anthraquinone (C.I.Disperse Violet 4), Isosorbide-5-Nitrae-diamino -2- methoxy anthraquinone (C.I.Disperse Red 11), 1- amino-2-methyl anthraquinone (C.I.Disperse Orange 11), 1- amino-4-hydroxy anthraquino (C.I.Disperse Red 15), Isosorbide-5-Nitrae, 5,8- tetra- ammonia Base anthraquinone (C.I.Disperse Blue 1), Isosorbide-5-Nitrae-diamino -5- nitroanthraquinone (C.I.Disperse Violet 8), C.I.Disperse Blue 7 etc. (being Colour Index name in bracket).
In addition to this it is possible to using C.I.Solvent Blue 14, C.I.Solvent Blue 35, C.I.Solvent Blue 63、C.I.Solvent Violet 13、C.I.Solvent Violet 14、C.I.Solvent Red 52、C.I.Solvent Red 114、C.I.Vat Blue 21、C.I.Vat Blue 30、C.I.Vat Violet 15、 C.I.Vat Violet 17、C.I.Vat Red 19、C.I.Vat Red 28、C.I.Acid Blue 23、C.I.Acid Blue 80、C.I.Acid Violet 43、C.I.Acid Violet 48、C.I.Acid Red 81、C.I.Acid Red 83、C.I.Reactive Blue 4、C.I.Reactive Blue 19、C.I.Disperse Blue 7、Sanodye Blue Pigment known to 2LW, Sanodye Blue G etc..
Above-mentioned anthraquinone pigments can be used alone or two or more is used in combination.In addition, in the present invention, by changing above-mentioned anthracene The type (molecular structure etc.) of Quinone Pigments can control detection sensitivity.
As methine class pigment, as long as the pigment with methine.Therefore, in the present invention, polymethine class Pigment, anthocyanins etc. are also contained in methine class pigment.These can be from known or commercially available methine class pigment In suitably use.Specifically, can enumerate C.I.Basic Red 12, C.I.Basic Red 13, C.I.Basic Red 14, C.I.Basic Red 15、C.I.Basic Red 27、C.I.Basic Red 35、C.I.Basic Red 36、C.I.Basic Red 37、C.I.Basic Red 45、C.I.Basic Red 48、C.I.Basic Yellow 11、C.I.Basic Yellow 12、C.I.Basic Yellow 13、C.I.Basic Yellow 14、C.I.Basic Yellow 21、C.I.Basic Yellow 22、C.I.Basic Yellow 23、C.I.Basic Yellow 24、C.I.Basic Violet 7、 C.I.Basic Violet 15、C.I.Basic Violet 16、C.I.Basic Violet 20、C.I.Basic Violet 21、C.I.Basic Violet 39、C.I.Basic Blue 62、C.I.Basic Blue 63、Sanodye Yellow3GL Deng.One kind or two or more be used in combination can be used in these.
Azo pigment, as long as there is no limit as the substance of chromophore with azo group-N=N-.For example, can arrange Lift monoazo pigment, polyazo pigment, metallic complex salt azopigment, talan azopigment, thiazolylazo pigment etc..More If being indicated with Colour Index name to body, can enumerate C.I.Solvent Red 1, C.I.Solvent Red 3, C.I.Solvent Red 23、C.I.Disperse Red 13、C.I.Disperse Red52、C.I.Disperse Violet 24、C.I.Disperse Blue 44、C.I.Disperse Red 58、C.I.Disperse Red 88、C.I.Disperse Yellow 23、C.I.Disperse Orange 1、C.I.Disperse Orange 5、C.I.Disperse Red 167:1、 C.I.Acid Red 18、C.I.Acid Yellow 23、Sanodure Fast Gold L、Sanodure Orange G、 Sanodye Red GLW、Sanodal Red B3LW、Sanodure Bordeaux RL、Sanodure Violet CLW、 Sanodure Green LWN、Sanodye Brown R、Sanodure Bronze 2LW、Sanodure Fast Bronze L、Sanodure Brown GSL、Sanodure Grey NL liquid、Sanodal Black 2LW、Sanodal Deep Black MLW、Sanodal Black GL Paste、Sanodure Fiery Red ML、Sanodye Golden Orange RLW, Sanodye Red RLW etc..One kind or two or more be used in combination can be used in these.
As phthalocyanines pigment, as long as there is no limit for the pigment with phthalocyanine structure.For example, the copper of blue can be enumerated The low chlorination phthalein of the more yellow green of phthalocyanine, the metal-free phthalocyanine that more partially green blue is presented, the high chlorination phthalocyanine of green, presentation Cyanines (bromination chlorinated copper phthalocyanine) etc..
Specifically, can enumerate C.I.Direct Blue 86, C.I.Direct Blue 87, C.I.Basic Blue 140, C.I.Solvent Blue 70, Sanodal Turquoise PLW Liquid etc..
In addition to above-mentioned general phthalocyanines pigment, can use with zinc, iron, cobalt, nickel, lead, tin, manganese, magnesium, silicon, titanium, palladium, The compound of metal centered at least one kind of in aluminium, iridium, platinum and ruthenium, these central metals and phthalocyanine complex, further with The compound of state and phthalocyanine complex etc. of bonded oxygen or chlorine on above-mentioned central metal.
As triphenylmethane pigment, as long as there is no limit for the pigment with triphenylmenthane structure.For example, can enumerate C.I.Acid Blue 90、C.I.Acid Green 16、C.I.Acid Violet 49、C.I.Basic Red9、 C.I.Basic Blue 7、C.I.Acid Violet 1、C.I.Direct Blue 41、C.I.Mordant Blue 1、 C.I.Mordant Violet 1, C.I.Acid Blue 9 etc..These triphenylmethane pigments, can be used a kind or 2 kinds with On be used in combination.
As xanthene class pigment, as long as there is no limit for the pigment with xanthene structure.For example, C.I.Acid can be enumerated Yellow 74、C.I.Acid Red 52、C.I.Acid Violet 30、C.I.Basic Red 1、C.I.Basic Violet 10, C.I.Mordant Red 27, C.I.Mordant Violet 25 etc..These xanthene class dyestuffs, can be used a kind or 2 kinds It is used in combination above.
As edible pigment, can and with edible Amaranth, edible No. 3 red, edible No. 102 red, edible red 104 Number, No. 105 edible red, edible No. 106 red, edible yellow 4, edible Sunset Yellow FCF, edible green 3, edible blue 1 Number, edible blue 2 etc..
In the present invention, the pigment or pigment in addition to above-mentioned pigment can be used together.Furthermore also can be used it is indefinite whether Belong to above-mentioned any pigment (ALFAST RED MF-301B, TAC RED BRL (being all trade name)).In particular, Pigment composition (claiming " non-discoloration pigment ") non-discolouring under plasma environment can be contained.Thus, it is possible to make from certain face The variation of tone of color to other colors is more made clear, and the visual recognition effect of discoloration can be more improved.It, can as non-discoloration pigment To use well known pigment, i.e., with dyestuff represented by trade name TAC BLACK-HG or Sanodal Gold 4N.Non- change at this time The content of color pigment can be suitably set according to the type etc. of the non-discoloration pigment.
But after being coloured in order to which indicator is made with above-mentioned pigment in the present invention, the common phase until before use Between, it is necessary to discoloration or colour killing cannot occur, will not be changed colour based on above-mentioned pigment or colour killing, the ageing stability of coloring are good.
[to the aluminium formed body surface by anodized after stain or non-coloring, or further across re-electrolysis The application of the pigment on the aluminium formed body surface of processing]
After forming hole on aluminium formed body surface by the above method, above-mentioned pigment is put into the hole.
Therefore, above-mentioned pigmentolysis is prepared into pigment solution in water or organic solvent, dipping passes through above method shape wherein At aluminium formed body made of hole.
As immersion condition, 1g/1L can be set as the pigment concentration in 2~30 minutes, 30~70 DEG C of temperature, pigment solution ~20g/1L.It washed, dried after dipping.
Processing in this way imports pigment 4 into hole as shown in Fig. 1 (b).Pigment has to be got over closer to aperture portion It fixes, more the tendency to the more a small amount of fixation in hole bottom more.Later can optionally carry out sealing pores makes the top of hole The opening portion in hole narrows.
[structure of indicator]
Indicator of the invention, the appearance of plate or foil-like with such as arbitrary size.At least the one of the one side of the plate The part coloured by dyestuff is formed on part.Such as the center of the one side of the substrate of rectangular plate can be formed in Part with dyestuff is coloured to circle, around do not have to dyestuff and coloured, carry out coloring or the processing of non-coloring alumilite process, into One step carries out the surface of re-electrolysis processing formation as needed.
But if dyeing is in circular situation, it is necessary to before dyeing process only leave circular portion in substrate surface setting and The masking component of masking.
The masking component can remove after dyeing process, can not also remove and the state to leave is as one of indicator Divide and uses.State to leave has in use, can not will pollute in plasma processing apparatus as far as possible in plasma loop Also the resin layer of Undec plasma-resistance can be used other sheet metals and sheltered as masking component under border. In addition, do not remove masking component and as indicator in use, the degree in order to confirm discoloration is optionally needed the masking The removal of dyestuff accompanying by parts surface.
Do not remove masking component and as indicator in use, in order to improve the visual recognition as indicator, preferably with phase Color and dyestuff for the state after being dyed with dyestuff decompose the color of the substrate of the state after removal, all can be abundant Ground confirms the color of color difference, and the material that will not change colour due to plasma colours masking component.
[purposes of indicator]
Indicator of the invention, as long as the corona treatment using the gas for generating plasma is all applicable in.I.e. for Low pressure plasma processing and atmospheric plasma treatment are all applicable in.
As the concrete example of low pressure plasma processing, for example, the cleaning of the flat-panel monitors such as liquid crystal display, surface can be enumerated The purposes such as modified；The purposes such as film, ashing, cleaning, surface modification in semiconductor fabrication sequence；Package substrate or printed circuit board Cleaning, the purposes such as surface is modified；The disinfectant applications of medical apparatus etc.；Purposes such as cleaning, the surface modification of encapsulating parts etc..
In addition, the concrete example as atmospheric plasma treatment, for example, the system of the flat-panel monitors such as liquid crystal display can be enumerated The purposes such as film, ashing, cleaning, surface modification；The purposes such as cleaning, the surface modification of package substrate or printed circuit board；Automobile flies The modified purposes in the surface of machine part etc., purposes such as disinfection, sterilization, sterilizing, treatment of medical field (dentistry or surgery) etc..
As the gas for generating low pressure plasma, as long as under lower pressure, by applying alternating voltage, pulse Voltage, high frequency, microwave etc. and can produce the gas of plasma there is no limit, for example, oxygen, nitrogen, hydrogen, chlorine, mistake can be enumerated Hydrogen oxide, helium, argon, silane, ammonia, sulfur bromide, vapor, nitrous oxide, tetraethoxysilane, carbon tetrafluoride, fluoroform, Carbon tetrachloride, silicon tetrachloride, sulfur hexafluoride, titanium tetrachloride, dichlorosilane, trimethyl gallium, trimethyl indium, trimethyl aluminium etc..This A little gases for generating low pressure plasma, can individually or two or more is used in mixed way.
As the gas for generating atmospheric pressure plasma, as long as under atmospheric pressure, by applying alternating voltage, pulse electricity Pressure, high frequency, microwave etc. and can produce the gas of plasma there is no limit, for example, oxygen, nitrogen, hydrogen, argon, helium, sky can be enumerated Gas etc..The gas of these generation atmospheric pressure plasmas, can individually or two or more is used in mixed way.
When using indicator of the invention, specifically, at the plasma using the gas for generating plasma Manage device (specifically, by containing generate plasma gas in the environment of apply alternating voltage, pulse voltage, High frequency, microwave etc. and the corona treatment implementing device for generating plasma) inside or its inner containment treated object It is upper to place indicator of the invention, it is exposed under plasma environment.At this point it is possible to by being placed in device The discoloration of indicator detects the implementation of fixed corona treatment.
Indicator of the invention can be used directly as instruction card.At this point, photochromic layer is shaped to well known The shape of bar code, as long as being set to that bar shaped can be passed through in the stage (degree of discoloration) that fixed corona treatment is completed The condition that code reader is read, so that it may the completion handled by bar code plasma and corona treatment object later Logistics management be managed collectively.Present invention could apply to indicators used in associated uses, corona treatment pipe Reason method and commodity distribution control method.
Indicator of the invention can be accommodated in the inside of gas permeability package body.
Gas permeability package body is preferably able to so that treated object is sealed in state therein and directly carries out corona treatment Package body.The known or commercially available object used as corona treatment with package body (bag) can be used in this package body Product.For example, being suitble to using the package body formed by polyethylene fiber (polyethylene synthetic paper).Treated object is put into the packaging Body can entirely be handled package body after being sealed to opening portion by heat-sealing etc. in plasma processing apparatus.
In addition to these situations, it can also be configured on the inner face of the package body.The method of configuration is simultaneously not limited, and removes base It, can also be by being directly coated with or being printed in package body for indicator of the invention except the method for adhesive, heat-sealing etc. Indicator is constituted on inner face.In addition, it is above-mentioned based on coating or printing in the case where, can package body fabrication stage with regard to preparatory Form indicator.
Then, in order to confirm indicator from outside, transparent window preferably is set in a part of package body.Example Such as, package body is made with clear sheet and above-mentioned polyethylene synthetic paper, in the position that can carry out visual recognition by clear sheet Set setting indicator.
It, can be using with for example when using storing the progress corona treatment of package body made of indicator of the invention Loaded into package body treated object process, to after filling treated object the process that is sealed of package body and should The method that package body is placed in the process under plasma processing environment.More specifically, after treated object being put into package body, It is sealed according to method well known to heat-sealing etc..Next the package body is entirely configured under plasma processing environment.Example It is such as configured in the process chamber of known or commercially available plasma processing apparatus, is handled.After treatment, package body is whole A taking-up can be taken care of directly in package body to when using.At this point, package body is preferably placed in plasma by corona treatment Until the photochromic layer of indicator changes colour under body processing environment.
Embodiment
[production of indicator]
(degreasing process)
Prepare JIS A1050 aluminium formed body, be impregnated in 50 DEG C, 6.5% sodium hydrate aqueous solution 3 minutes, washes, into one Step is impregnated in 10% nitric acid at room temperature and is neutralized for 3 minutes, is cleaned with ion exchange water and carries out degreasing.
(anodized process)
Prepare 15% sulfuric acid as electrolyte, the aluminium formed body after degreasing is impregnated in the electrolyte, direct current Constant Electric Current is passed through Solution is electrolysed.It is used as using carbon plate to electrode.
In electrolysis, current density 1.0A/dm2, bath temperature is 20 DEG C, and electrolysis time is 40 minutes.
(dyeing process)
In the dye solution of the dye strength 5g/L, pH5.5, temperature 50 C that are obtained using dyestuff shown in table 1, dipping Aluminium formed body by anodized 10 minutes.Temperature or time when by change dye strength, pH, dipping, can be with Adjust the concentration of the color obtained by dyeing.
In addition, by changing the electrolytic condition in anodic oxidation process, the also concentration of the adjustable color obtained by dyeing.
[high-frequency plasma processing]
Will the indicator made of above-mentioned operation, be set in plasma processing apparatus.
Later, by the following conditions, O is used only2Gas and use O2Gas and CF4The mixed gas of gas generates plasma, makes Pointer detection plasma.
(high frequency O2Plasma process conditions)
Using parallel plate-type high frequency plasma body device BP-1 (Samco Co. Ltd. system), O is supplied with 10ml/min2Gas, Simultaneously under the air pressure of 100Pa, 50mm is set by interelectrode distance, 30 minutes corona treatments are implemented with 100W.
(microwave O2Plasma process conditions)
Using microwave plasma device (TMP-0063 (Toshiba Corporation's system)), O is supplied under 2.5Torr air pressure2Gas, The power of 1kW is supplied, initial stage low pressure is 0.95Torr, and initial stage temperature setting is 30~33 DEG C, is implemented at 30 minutes plasmas Reason.
(high frequency O2And CF4Plasma process conditions)
Using parallel plate-type high frequency plasma body device BP-1 (Samco Co. Ltd. system), O is supplied with 10ml/min2Gas, CF is supplied with 5ml/min4Gas, while under the air pressure of 100Pa, 50mm is set by interelectrode distance, is implemented with 100W 30 minutes corona treatments.
[assessment]
(color change when plasma detects)
To the color before and after detection plasma visually to confirm.
(discoloration)
The indicator that will test the front and back of the process of plasma discharges side by side, the degree to be changed colour with visual confirmation.
The indicator zero that can be changed colour with visual confirmation
With not can confirm that visually the indicator of discoloration ×
(time-varying of discoloration)
After placement indicator 4 weeks, the assessment of above-mentioned discoloration is carried out in 50 DEG C.
The indicator zero of discoloration identical with initial stage can be confirmed
It is reduced with preliminary phase than discoloration, but the indicator △ of discoloration can be confirmed
The indicator-of time-varying is not can confirm that
In embodiment 1~19, will by various alumilite process processing substrate, by after various dyeings for etc. The detection of gas ions.
The Comparative Examples 1 to 5 will by various alumilite process handle but without pass through dyeing, or using inorganic salt dyestuff into The substrate of row dyeing is used for corona treatment.
[table 1]
According to the embodiment 1~19 of above-mentioned table 1, when using aluminium sheet by dyeing, based on high frequency and microwave etc. from Daughter all detects and changes colour.
On the other hand, it according to dyeing, or the Comparative Examples 1 to 5 dyed using inorganic salt dyestuff is not passed through, does not send out Change color.
In addition, according to embodiment 1~19, and aluminium formed body of having no way of releases the sign of which kind of substance into plasma environment.
The substrate of embodiment 1~19 is before alumilite process processing, or can be used in the way of each process of coloring commercially available Masking material assign style appropriate, the design of indicator can be improved.As masking material, wild pharmacy work difficult to understand is being used When the Topresist1000 of industry Co. Ltd. system, a part use of masking material and the composition as indicator is not removed The adverse effect based on corona treatment is not observed.

Claims (3)

1. a kind of alumilite process containing pigment handles plasma indicator, which is characterized in that make by anodic oxidation Reason and the hole formed contain pigment and form.
2. the alumilite process according to claim 1 containing pigment handles plasma indicator, which is characterized in that color Element is selected from anthraquinone pigments, methine class pigment, azo pigment, phthalocyanines pigment, triphenylmethane pigment, edible pigment And it is at least one kind of in xanthene class pigment.
3. the alumilite process according to claim 1 or 2 containing pigment handles plasma indicator, feature exists In the hole is formed through sealing pores.
CN201780080935.7A 2017-01-04 2017-12-26 Alumilite process containing pigment handles plasma indicator Pending CN110114668A (en)

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