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? Method of manufacturing electret 0 Application No. FIPJ 45-115095 [Phase] Application
Akira 45 (1970) December 22 @ inventor Kunitomo Tetsunosuke Otsu City Oyama 2 10 10 Ueno
Takahiko Town Takamiyacho 2365 same Fujioka Shuji Otsu City Oyama Detailed description of
two inventions of 10 applicants 2 of 10 Masao Iwamoto Otsu City Sonoyama 2 east of
Nihonbashi Muro-cho Chuo-ku, Tokyo The present invention relates to a method of
manufacturing electrets, and in particular positive and negative The present invention relates to a
method for producing a polyvinyl chloride or chlorinated polyethylene electret having a high
charge amount and a long life. Conventionally, various electrets made of synthetic polymer
substances have been developed in general, but it is probably due to the electretization method
(thermal electretization) that the material itself is denatured, and even if it is electretized, the
charge amount itself is also It was extremely low, and the time loss of charge was large, and the
practicability was extremely small. In particular, the polyvinyl chloride electret obtained by the
above-mentioned conventional method has a large alteration of the material itself, and the charge
amount is at most 100 volts at surface potential and at most 10 "-'to 10" 0 Coul / cIrL2 in
surface charge density. . In addition, methods of producing electrets having negative charges on
both sides by electron beam irradiation are already known for polytetrafluoroethylene,
polyethylene terephthalate, and polycarbonate CG, M. [111111] 5essler, J @ E, Westt J-Polymer 5
et pt B 7 (5) 367 (1970)), it is not known to make electrets of different charge codes on both
sides by this method. Therefore, the present inventors conducted investigations to solve these
conventional methods. For that purpose, we reached the theory of the result of conducting
detailed study aiming at the development of high charge, high life and long life, and the result
that both the charge of ? and the charge were effective. Then, the method of achieving this was
firstly selected as a suitable material, and as a result of extensive examination of the concrete
method, the following materials and methods were found and the invention was reached. That is,
the present invention is characterized in that a film or sheet of polyvinyl chloride or chlorinated
polyethylene having a volume resistivity of 10 13 ? и ? or more placed on an electrical insulator
is irradiated with an electron beam. The present invention provides a method for producing an
electret in which the irradiation surface is positively charged and the opposite side is negatively
charged. In the present invention, the electrical insulator preferably has a volume resistivity of
10 13 ? и ? or more, and the object of the present invention can not be achieved with poor
electrical insulation.
The material is not particularly limited as long as it is such, but, for example, various organic
polymer substances such as polyethylene, polypropylene, polystyrene, polytetrafluoroethylene,
polycarbonate, polymethyl methacrylate, etc., inorganic materials such as glass and ceramics, and
composites of both There is a material etc. The purpose can not be achieved with ordinary metal
materials and the like. The polyvinyl chloride used in the present invention may contain other
minor components by copolymerization or the like to such an extent that the properties thereof
are not impaired. Chlorinated polyethylenes having a known degree of chlorination (40 to 70%),
mainly those having a degree of chlorination equivalent to polyvinyl chloride (57% by weight),
are used. These polyvinyl chlorides or chlorinated polyethylenes must have a volume resistivity
of 10 13 ? и ? or more [111111] EndPage: 1 is required. The polyvinyl chloride or chlorinated
polyethylene used in the present invention is formed into a film or sheet, but those formed into
an envelope or the like may also be used. When forming and processing this film or sheet, it is of
course necessary to have, for example, a molecular weight, dissolution or solution #I resistance
to endure the formation processing, but after forming it becomes insoluble and infusible Not only
that, but sometimes it is preferable to suppress charge decay. The molecular weight is preferably
at least 500 or more in average polymerization degree. The forming method is not particularly
limited. For example, any of solution method and melting method can be used, and examples of
the former are solvents such as dioxane, ethylene dichloride, methylene dichloride,
cyclohexanone, dimethylformamide and tetrahydrofuran There is a method of melting and
casting, and examples of the latter include compression molding, injection molding, extrusion
molding, calendering method and the like. A plasticizer, a stabilizer, a filler, a colorant, an
antistatic agent, a flame retardant, etc. can be added in the process of molding or prior to
molding, but the important thing is that the electrical resistance of the molded product obtained
That is, the addition amount must be adjusted so that the volume resistivity does not become
lower than 10 13 ? и ?. Examples of plasticizers used for polyvinyl chloride and chlorinated
polyethylene not subjected to internal plasticization include di-2-ethylhexyl phthalate (DOP), di-noctyl phthalate (n-DOP), tricresyl phosphate ( TCP), dioctyl sebacate (DO8), etc. are relatively
Moreover, as a stabilizer, although lead salt type, metal soap type and organic tin compound type
are mainly used, the large amount of addition of such a stabilizer was limited to about 5% (by
weight) to reduce the electric resistance value. One is better. This is also true for the antistatic
process. The sheet may be any of non-stretching, -axial stretching, and biaxial stretching, but in
the case where the obtained electret is expected to have piezoelectricity, it is preferable to use a
sheet subjected to a stretching treatment. Although the thickness of the sheet is finally
determined in relation to the irradiation amount, it is desirable to make the thickness of the sheet
1 1000 ?m or less in order to use under the irradiation conditions described later, and the
[111111] sheet is overlapped and irradiated Also in this case, it is preferable that the total
thickness is 5 mm or less. Examples of electron beam generators usable in the present invention
include the Kokkokcroft-type accelerator, the Kotokcroft-Walton-type accelerator, the Pan-degraph-type accelerator, the pressure booster, the linear accelerator, the betatron, the
dynamidron-type accelerator, the iron core insulation There is an accelerator etc. It is preferable
that these electron beam generators generate energy of about 150 Kev or more. Next, the actual
electretization will be described. The irradiation dose varies depending on the radiation
resistance of polyvinyl chloride or chlorinated polyethylene to be electretized, the size of the
charge amount to be obtained, and the like, but a range of 0.01 to 50 Mrad is desirable. The
irradiation time varies depending on the accelerating voltage, the beam current, etc., but in order
to prevent deformation or breakage of the film or sheet (which may be a molded product
thereof), it should be at most several seconds. Irradiation can be performed in air, at normal
temperature and normal humidity, but can also be performed in vacuum or in nitrogen or argon
gas, and heating at the time of ? irradiation, or simultaneous irradiation with light such as xenon
light or a mercury lamp You can also. An electric insulator is applied to polyvinyl chloride or
chlorinated polyethylene molded into a film or sheet, and the electron beam is directly scattered,
but in this case polyvinyl chloride or chlorine to be electretized t The distance between the
polyethylene oxide and the electrical insulator should be 16 IIL or less. Preferably, it is better to
adhere closely. Also, the present invention achieves the moonly effect only when the electric
insulator is used and irradiation is performed on the side opposite to the irradiation side of the
polyvinyl chloride or chlorinated polyethylene film or sheet irradiated with the electric insulator.
It is quite surprising that the number of cases has to be such a method, which is currently
In addition, when irradiating to an envelope-like molded object, it irradiates in the state in which
an electric insulator is stuck inside. ? The features of the present invention can be understood
from the above explanation The main features of the invention are: (1) There is no deterioration
or deformation of the material itself during electretization as seen in the conventional
electretization operation, and it is simple Having developed a unique way. [111111] EndPage: 2
(2) The electret obtained has positive and negative charges on the irradiated side, which is a
novel fact not found at all in the conventional electret field, Greatly encourage the development
of electrets. (3) The electret obtained by the development of the above new technology has a very
high charge amount, a surface potential of about 1000 volts or more, and a surface charge
density of 10 ? ? ? 6 to 10-7 (CculA2). It is one to several orders of magnitude larger than
one. (Conventional method: 100 volts or less 1.10 -9 to 10 -10 Coul / cIrL2) (4) Also, electrets
that give such high charge have a slowing rate, and it is almost initial charge even after 3
months. Is the same as It was also confirmed that even if this electret was immersed in water or
an aqueous electrolyte solution, its reduction was small. Furthermore, it has the property which
can not be seen conventionally, having piezoelectricity. It is noted that further reduction of the
degree of this reduction according to the invention is possible with the choice of modified
polyvinyl chloride. (5) It should be noted that the present invention is particularly unique only to
polyvinyl chloride and chlorinated polyethylene having a volume resistivity of 10 13 ? и ? or
more, for example, even if it is similarly applied to low density polyethylene (10 16 ? и crIL). It
becomes more obvious from the fact that it does not. From the above characteristics, the electret
of the present invention not only extends the conventional application, but also opens up new
application fields. For example, acoustic devices such as microphones, pickups and speakers,
electronic copying and printing applications, medical materials, especially materials for
instruments that contact blood, etc. . ????? The measurement method of the electrical
properties of the XV Tactto shown in the invention 38 'is as follows. ? Volume specific
resistance: It measured based on JIS standard using Takeda Riken HighVoltagePower5upplyTR =
300B, TR'-84B, VltraHighMegohmmeter, and SampleChamberTR-42.
? Surface potential: The Koa Shokai rotary static tester was used. Although this device was
originally made to measure Masatsu [111111] static electricity, it was used without installing a
Masatsu object. The sign of the charge was determined from the waveform by mounting a
synchroscope on a storage device. (2) Surface charge density: The following two methods were
used. Parallel plate capacitor method: From surface potential VA (bolt) measured by sticking
copper foil to the sample fixing point of Koa Shokai rotary static tester and making the back of
the sample grounded, and dielectric constant ?S measured separately 0 calculated by the
following formula: where d is the thickness of the film or sheet, cm). In addition, (epsilon) S is the
value calculated | required using direct current by the method described in "physics
measurement technique 1st volume (breakfast bookstore) p, p114-147. Depolarization current
method: Takamatsu [fiber and industry 2 (the fiber and industry 2 (the fiber and industry 2) by
integrating the amount of current flowing through the circuit and dividing it by the area of the
electret sample when heating the electret with both sides of the electret shorted. 9) The method
of 649 (1970) was applied as it was. Example 1 Hoshi-made Hori vinyl chloride film 6 Neufan
"(biaxially stretched, 25?), affixed to a glass plate, normal temperature always! The electron
beam was irradiated using a pan-de-graph type accelerator in the lower air. The acceleration
voltage was IM eV, the beam current was 100 ?A, the belt travel speed was 8 cIrL / min, and the
irradiation amount was 5 Mrad. Remove film after irradiation, 20 ░ C, 6! 5% RH constant
temperature and humidity for 24 hours, remove the influence of static electricity by means of an
apparatus and remove the surface potential by the method described in the main text. Irradiated
surface is +950 V; Met. The gloss surface charge dense saponification calculated by the concept
of the parallel plate capacitor method is 1. ?????? coul / cm 2, determined by
depolarization current method, k was 5 О 10 ?7 coul / c IrL 2. Cono electrets have X, 1 иии with
a charge of + 840 V and an opposite side of + 840 V after 3 days. The electret was immersed in
water and 0.9% [111111] EndPage: 3 saline solution for 2 days after preparation, and then air-
dried to determine the surface potential). It recovered up to 500 volts two days later. It is to be
noted that this electret was found to have piezoelectricity [111111] Example 10 Three sheets of
the film used in Example 2 were stacked and placed on a polymethyl methacrylate plate, and this
was irradiated with 5 Mrad of electron beam. Under various conditions substantially the same as
those in Example 1 and Example 2, the following polyvinyl chloride films were attached to a
polymethyl methacrylate plate and irradiated with an electron beam of 5 Mrad.
Table 1 shows the results. . ????????? The leftt was obtained. The surface potential was
the same for all three and was about 1,000 volts. Examples 11 to 16 The conditions are changed,
an electron beam of 5 Mrad is irradiated, and the results in Table 2 are as follows: 111EndPage:
4 * +: those which can be electretized; Examples 17 to 22 r [111111] Example 23 The film of
Example 9 was adhered to a polyethyl methacrylate plate and irradiated with 5 Mrad of electron
beam in nitrogen gas to give about 500 Electret of bolt is Tokimine ? 1111]
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