The way nonelectrolytic plating aramid surfaces

 

(57) Abstract:

Describes how nonelectrolytic plating aramid fibers with durable coating metal coating, comprising contacting aramid fibers with acid solution for at least 2 at a temperature in the range of 10 to 100°C., washing with water to the practical removal of all acid, contacting the fibers with an activating solution, rinsing and immersion in a solution of cations of deposited metal, characterized in that the acid solution using a solution selected from the group comprising 86-91 wt.%-percent aqueous nitric acid, 1-5 wt.%-percent chlorosulfonic acid in an organic liquid and 1-5 wt.%-ing persulfonic acid in the organic liquid. The technical result is an increase in the rate of metallization with preservation of the fibrous product, almost retained the strength and modulus of elasticity, a metal coating which is highly conductive and high adhesion. 3 C.p. f-crystals, 2 tab., 2 Il.

Background of the invention

The technical field to which the invention relates

This invention relates to a nonelectrolytic plating of aramid fibers in bone. The aramid is subjected to pre-processing before the metallization, including carefully controlled exposure to a concentrated aqueous solution of nitric acid or in dilute solution of chlorosulfonic or persulfonic acid in the organic liquid, followed by washing, catalysing and nonelectrolytic plating.

Description of the prior art

Nonelectrolytic plating is the deposition of metal film in the interaction of metal ions and agent chemical recovery in the alkaline solution. Nonelectrolytic plating in General is well known. One of the difficulties in achieving successful nonelectrolytic plating is to obtain good adhesion between metaliteracy substrate and the deposited metal. Although only encapsulation may be sufficient for some applications and some products, good adhesion of deposited metal is essential to the surfaces of the fibers, because the deposited metal coating should be robust enough to withstand further processing and stresses the final application.

U.S. patent No. 5 is processing before the metallization, using 80-90% aqueous solution of sulfuric acid.

Brief description of the invention

The present invention represents a method for metallization of aramid fibers at the increased speeds metallization durable metal coating, comprising the stage of: extracts of aramid fibers in the acid solution 86-92 wt. % aqueous nitric acid or 1-5 wt.% chlorosulfonic acid or persulfonic acid in the organic liquid for at least 2 at a temperature in the range from 10 to 100oC, washing and neutralizing acid etched fibers with water up until practically all the acid is removed, and bonding fibers nonelectrolytic way metallization.

For the metallization of the fiber copper process nonelectrolytic plating can be carried out while contacting the acid-treated and washed fibers with a tin-palladium activating solution, washing the fibers in water to remove leatheireannach metal, optional, immersing the washed fibers in aqueous accelerating solution of mineral acid, and then immersing the fibers in a bath nonelectrolytic plating copper.

When you practice on the La silver coating.

Brief description of drawings

Fig. 1 is a micrograph with a magnification x 500 fibers, poorly plated.

Fig. 2 is a micrograph with a magnification x 500 fibers treated in accordance with the present invention.

Detailed description of the invention

Long ago, there is a need for conductive aramid fibers, which have a durable metal coating; and this need is especially acute for fibers which have high strength and modulus of elasticity.

Fibres of aramids are very difficult to cover durable metal coating. Processing and pre-processing the surface of the aramid fibers are generally not completely satisfying.

This invention represents a method for nonelectrolytic plating fibres of aramids at greatly increased speeds metallization, which in some ways gives metallized fibrous product, almost retained the strength and modulus of elasticity, and a metal coating which is highly conductive and high adhesion. The method can be implemented on a continuous basis or periodicscanretry to two aromatic rings. Appropriate aramid fibers are described in Man-Made Fibers: Science and Technology, Volume 2, Section titled Fiber-Forming Aromatic Polyamides, p. 297, W. Black et al. Interscience Publishers, 1968. Aramid fibers are also discussed in U.S. patent 4172938, 3869429, 3819587, 3673143, 3354127 and 3094511.

With aramid can be used additives, and, as a special case, it was found that up to 30 wt.% the polyvinylpyrrolidone may be introduced into a poly(p-phenyleneterephthalamide) aramid fibers, metallized method of the present invention.

Para-aramids are the primary polymers in the fibers of this invention and poly(p-phenyleneterephthalamide) is the preferred para-amidon. Under the poly(p-phenyleneterephthalamide) refers to a homopolymer, the resulting mole-for-mole polymerization of p-phenylenediamine and terephthaloylchloride, as well as copolymers obtained by the addition of small amounts of other diamines with p-phenylenediamine and small amounts of other chlorides of dibasic acids with terephthaloylchloride. As a rule, other diamines and other chlorides of dibasic acids may be used in amounts up to about 10 mol.% p-phenylenediamine or terephthaloylchloride or perhaps a bit large only on the condition that other diamines and chlorides dogoftheday) also means copolymers, resulting from the introduction of other aromatic diamines and other aromatic chlorides of dibasic acids, such as, for example, 2,6-naftanaila or chlorine - or dichloro-terephthaloylchloride, provided only that the other aromatic diamines and aromatic chlorides of dibasic acids are present in quantities which provide an anisotropic spinning "syrups". Obtaining p-phenyleneterephthalamide described in U.S. patent N 3869429, 4308374, 4698414.

The fibers of this invention can also be used in meta-aramids, poly(m-phenylenedimaleimide) is the preferred meta-aramid. Under the poly(m-phenylenedimaleimide) is meant the homopolymer resulting mole-for-mole polymerization of m-phenylenediamine and isophthalonitrile, and copolymers resulting from the introduction of small amounts of other diamines with m-phenylenediamine and small amounts of other chlorides of dibasic acids with softlogica. As a rule, other diamines and other chlorides of dibasic acids may be used in quantities of up to 10 mol.% m-phenylenediamine or isophthalamide or maybe a little larger, provided only that the other diamines and chlorides of dibasic acids do not have the copolymers, resulting from the introduction of other aromatic diamines and other aromatic chlorides of dibasic acids, provided only that the other aromatic diamines and aromatic chlorides of dibasic acids are present in amounts that do not impair the desirable characteristics of aramid.

Aramid fibers obtained wet or air ways spinning of the above patents, are coagulated in the so-called "non-drying" form, in which the fiber contains significantly more than 75 wt.% water. "Non-drying" of the fibers are then dried to less than about 20 wt.% water in order to destroy the polymer fiber structure. Fibers suitable for use in the method of the present invention are dry fibers having a moisture content less than 20 wt. %. Typically, the fibers used in the method of the present invention, should be even more dry, having a moisture content of about 3.5-7% of water.

In the first stage of the method of the present invention metallized aramid fiber in contact with the acid pre-treatment. Acid pre-treatment used in the implementation of the present invention, is an aqueous nitric acid or chlorine - or ptors the I acid, no water phosphoric acid does not give acceptable results when used as the acid pre-treatment; it was found that chlorine - and persulfonic acid dissolve in water and should be used in non-aqueous liquid.

Pre-treatment of the present invention can be carried out using aqueous nitric acid concentration of from about 86 wt.% to the concentration where there is excessive danger for the processed material. The limits of concentration of the acid, of course, depend on the temperature and duration of pre-treatment. Pre-treatment is usually carried out at ambient temperature, typically 20-40oC, and if the average duration is typically 5-60 C. If the temperature or the duration of pre-treatment increased the concentration of acid may be correspondingly reduced. At higher temperatures or increased duration can be effective nitric acid concentration of less than 86 wt. %, while at lower temperatures or reduced duration can be used nitric acid concentrations of more than 86 wt.%. When the acid is too low concentration, has preliminarily the acid is too high concentrations, the treated fibers are excessively destroyed.

For pre-treatment of the present invention chlorosulfonic acid and persulfonic acid are used in relatively dilute concentrations in the organic liquid. Organic liquids which are suitable for use include any which are mixed acids and acid do not react. Examples of such liquids include methylene chloride, hexane, cyclohexane, etc., the Concentration of these haloalkaliphilic acids for pre-treatment of the present invention should be from about 1 wt.% to the concentration where there is excessive risk for processed materials, about 5 wt.%. Conditions pre-treatment using these haloalkaliphilic acids usually are the same as for aqueous nitric acid.

Pre-treatment of aramid fibers using the above-described acids at given concentrations, durations and temperatures gives extremely fast set speed metallization, as will be shown in the following Example. Although the reason for this speed dial speed fully nevyyasneno, it is clear that the processing and the Oh at concentrations of 1-5% at a temperature of 30oC gives a set speed metallization aramid fibers, which increases sharply.

The temperature of the bath of acid pre-treatment must be in the range from 10 to 100oC, preferably about 20-40oC. the Upper temperature limit is determined by the harmful effects on the mechanical properties and the fusing filament yarn, whereas the lower temperature limit is a matter of expediency: lower temperatures require unacceptably long time for adequate processing.

Fiber, which may be of any desired thickness, in contact with the acid for at least 2 sec. At shorter exposure times are hard, ultimately, to achieve sufficient depth. A longer exposure time at the same time gives excessive cracking of elementary fibers and causes loss of strength properties. Typically, the contacting fibers with acid for more than 120 seconds even at moderate temperatures leads to the destruction of the fibers. The preferred contact time is about 15-40 C. the exposure Time in the acid can be reduced by increasing temperature and/or increasing concentration of acid. Effective implementation is the etching duration.

Stage acid etching method of this invention makes the surface of the etched fibers and causes structural changes and cracks formed on the surface of the fiber. On the accompanying drawings Fig. 1 is a micrograph of fibers of poly (p-phenyleneterephthalamide), which were immersed for 20 to 85 wt.% nitric acid at a temperature of about 20oC, and Fig. 2 is a micrograph of fibers of poly(p - phenyleneterephthalamide), which were immersed for 5 to 90 wt.% nitric acid at a temperature of about 20oC. Fiber in Fig. 1 are smooth and do not have prominent changes during processing, while the fiber in Fig. 2 are cracked and uneven delamination along its length. The processing shown in Fig. 1, is inadequate to produce metallic coatings with high adhesion of the present invention; and the processing shown in Fig. 2, gives the desired adhesion of the metal.

An important aspect of the present invention is that the pre-processing uses acid under conditions that really change the structure of the fibers in order to achieve the desired adhesion of the deposited metal. Although the change is supported on the stage is 2">

Etched acid fibers of poly (p-phenyleneterephthalamide) well washed with water to remove practically all of the acid. Optionally, the fiber may be neutralized with base such as sodium bicarbonate solution, which can be added to washing water or used in a separate stage. You can also dry etched by acid fiber to the stage metallization.

The essence of this invention lies in the discovery that aramid fibers, treated with acid as described herein may provide improved metallized fibrous product. As a rule, well-known methods nonelectrolytic plating can be used for metallization of aramid fibers after acid treatment in accordance with the present invention.

For example, for a method of copper metallization aqueous activating solution is obtained by using cations of palladium and tin as catalyst activation. Metallized acid etched and washed fibers of poly (p-phenyleneterephthalamide) are immersed into the solution and mixed to ensure activation of the surface of the fibers. Then the fibers, if necessary, removed from antiviruse the mineral acid.

The fibers are then placed in or passed through a bath of plating with copper ions and formaldehyde, where the copper ions form a complex with keeping them in solution, for example, with TETRANITRATE salt of ethylenediaminetetraacetic acid (EDTA).

When implementing the present invention can be used in the bath, with a wide range of concentrations of the metal. The preferred metallization baths contain about 1-5 g/l of copper. In the experiments described here, the most preferred are baths with 1-3 g/l of copper.

Bath plating from deep in the fibers moderately stirred for 10-20 min to ensure adequate growth. When the speed reduction is added formaldehyde, pH-adjustment alkaline solution and the solution with copper ions. Add run continuously or intermittently. The metallic material can then be washed and dried. As reducing agents instead of formaldehyde can be used other materials. Suitable reductants are hypophosphite, hydrazine, boron hydride, etc.

All of the above stages can be conducted in different baths at temperatures from 10 to 60oC, preferably 2 is ruhut in an aqueous solution of a reducing agent, such as SnCl2/HCl. Immersed in SnCl2/HCl fibers are washed thoroughly with water to remove excess and leatheireannach ions of divalent tin and then transferred to a water bath to which is added metalcomplexes solution of silver nitrate and ammonia baths at pH 8-9,5. In the process of immersion in metalcomplexes tub last mixed to ensure that the absorbed ions of divalent tin restored silver ions to silver preferred deposition on cerebrocurin polymer surface. In a typical method, the molar ratio of formaldehyde: silver is from 1.1:1 to 2:1. The amount of silver nitrate is regulated to provide the desired mass of recovered silver as a function of the metallized fibrous material. Metallic silver fibers are washed and dried.

Instead of silver or copper, Nickel or cobalt, or the like can also be applied to acid etched fiber with its own combination of the activating solution, the solution of the reducing agent and the metallization solution.

The processes of metallization can be carried out on the acid etched fibers, which metallization relatively unnoticed effect drying of the fibers after contact with the acid. However, the process of silvering gives the output of deposited silver with the lowest resistance when the fibers are first dried at a temperature of about 15-80oC, preferably 15-20oC. When metallic silver fibers are dried at medium heat, significantly less penetration of metallic silver in the fibrous structure than for the wet fibers, and celebrated the best continuous silver coating than is realized for fibers, asepsis at higher temperatures.

Test methods

Resistivity

The resistance element is constructed by installing copper electrodes with a length of 25.4 mm in parallel and 25.4 mm per side on a flat block neprovedenija, such as polyethylene. The electrodes are connected with an ohmmeter, such as the multimeter Katli A, and the resistance of the tissue is determined when the pressing element to tissue located on a flat non-conductive surface. The fixed resistance in ohms per square.

Description of the preferred options

Getting metallized fibers.

In the Example below, use the following.

Metallized fibers or first processed by acid the ATEM processed by acid pre-treatment. Of course, the fibers for the comparative examples are not subjected to acid treatment or treated with acid outside the interval of concentrations or conditions required by this invention. Used knitting machine brand COMETS firm Scott & William, Laconia, new Gempar, USA, having a head diameter 8,89 cm (3,5 inch); the result is a fabric consisting of six rows (stitches parallel to the axis of the cylinder) and the five fingered columns (stitches perpendicular to the axis of the cylinder).

Each of the samples knitted fabric is then subjected to a nonelectrolytic plating of copper using commercially available chemicals as follows:

(a) contacting tissue within about 10 minutes at a temperature of approximately 40oC with an aqueous activating solution of mineral acid, chloride of divalent tin and palladium, for example a solution of 60 ml "Catatonic" 44 firms Shipley To. and with an aqueous solution of sodium chloride and tin, for example a solution of 540 g "Dataprep" 404 firm Shipley To. in 1700 ml of water to obtain a palladium-tin complex to activate the surface of the fibers;

(b) rinsing the yarn for about 5 minutes with two changes of water at temperature metallization, containing, for example, 240 ml "Circuit" M company Shipley and Co. , 84 ml "Circuit" A company Shipley and Co., 200 ml "Circuit" V company Shipley and Co. and 1476 ml water;

(d) rinsing the yarn for about 7 min in two changes of water at a temperature of approximately 25oC and

(e) drying the yarn until the morning in the vacuum heating Cabinet at a temperature of about 20oC.

"Circuit3350M" is a trademark of the company Shipley To. to a solution of 25 wt. % ethylenediaminetetraacetic acid and 75 wt.% water and safe materials.

"Circuit3350A" is a trademark of the company Shipley To. to a solution of 7 wt. % formaldehyde, 10 wt.% copper sulfate, 3 wt.% hydrochloric acid and 80 wt.% water and safe materials.

"Circuit3350B" is a trademark of the company Shipley To. for solution of 5 wt.% sodium hydroxide, 95 wt.% water and safe materials.

For the purposes of these examples, the analysis of the metallized fibers on metallic copper to determine the amount of copper deposited in the metallization process.

Example 1 and Comparative examples 1-4

In these examples, the effect of nitric acid as the acid pre-obra filament (445 decitex, with 1.7 dtex per filament) made from poly(p-phenyleneterephthalamide) and delivered by the company E. I. du Pont de Nemours & company under the trademark "KEVLAR"29.

Yarn spun from fibers treated by immersion in nitric acid at a temperature of about 20oC at the concentrations and duration specified in Table 1; then thoroughly washed with water and immersed in a 8 wt.% the sodium bicarbonate solution for 5 min before washing in water again for an hour and a half. Etched yarn is dried in the air and made from it a tube that metallizers in accordance with the above-described method.

In Table 1 data on the increase of copper (expressed in wt.% metallized fibers) and resistivity show that nitric acid at 20oC is effective at concentrations above 85% for pre-treatment of the fibers to provide metallization copper. The concentration of nitric acid 85% is effective at a slightly higher temperature pre-treatment to approximately the 50oC; and 86 wt.% can be used effectively at 20oC. the Data in Table 1 also show that pre-treatment esotropia, as indicated by the absence of copper particles during visual analysis of the wash water metallization. The presence of copper particles in the wash water metallization is a sign of poor adhesion of copper to a fibrous substrate: the more particles, the worse adhesion.

Comparative example 5.

In this example, the effect of phosphoric acid as the acid pre-treatment.

The same aramid yarn that was used in the previous examples, is treated aqueous phosphoric acid in a concentration of about 87 wt.% 60 seconds according to the method described in Example 1. The acid-treated yarn is neutralized, washed, processed into small fabric sleeves and metallservisa copper according to the method described above. The growth of copper on tissue sleeve is equal to only 23.3 per cent. The fabric sleeve is covered with a copper unevenly, and the electrical resistance of the fabric is equal to more than 3108Ohms/square, This example shows that pre-treatment of aramid yarn highly concentrated phosphoric acid does not contribute to the metallization of copper compared with the influence of pre-treatment with nitric acid is approximately equal conc the new acid as the acid pre-treatment.

Aramid yarn of the previous examples are processed into small tissue sleeve in accordance with the above-described method; and the yarn is pre-processed in the form of sleeves. The terms of the preliminary processing of the sleeves before the metallization is provided in Table 2. The data show that 2 wt. % chlorosulfonic acid (ClSO3H) in any of the methylene chloride, hexane or cyclohexane has a different effect on the growth of copper and resistivity. When using pre-treatment chlorosulfonic acid is not observed copper particles in the wash water after metallization.

Chlorosulfonic acid can be used as an effective pre-treatment at such a low concentration as 1 wt.% any organic liquid that is miscible, but does not react with acid. Temperature pre-treatment is normally around the 20oC activity increased with increasing temperature and duration of pre-treatment is usually less than 60 C. When the acid concentration of more than 5 wt.% aramid fiber can significantly impair the strength properties in the pre-treatment at too Getsa for pre-treatment in the same manner and under the same conditions, as chlorosulfonic acid.

Comparative example 8

In this example, the effect of hydrochloric acid as the acid pre-treatment.

Aramid yarn of the previous examples are processed into small fabric sleeve as described above. The yarn is pre-processed in the form of sleeves aqueous hydrochloric acid concentration of about 38 wt.% within 60 minutes at a temperature of about 20oC. the acid-Treated sleeve is then neutralized, washed, dried in air and metallservisa copper according to the method described in Example 1. The growth of copper on tissue sleeve is only 26 wt.%, and the resistivity is equal to more than 3108Ohms/square

1. The way nonelectrolytic plating aramid fibers with durable coating metal coating, comprising contacting aramid fibers with acid solution for at least 2 at a temperature in the range of 10 - 100oC, the washing water to the practical removal of all acid, contacting the fibers with an activating solution, rinsing and immersion in a solution of cations of deposited metal, characterized in that the acid solution used in the second acid in the organic liquid and 1 - 5 wt.%-ing persulfonic acid in the organic liquid.

2. The method according to p. 1, wherein prior to contacting the fibers with an activating solution dried them.

3. The method according to p. 1, wherein the durable metal is copper or silver.

4. The method according to p. 1, characterized in that the activating solution is a tin-palladium solution or a solution containing bivalent tin.

 

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FIELD: textile, paper.

SUBSTANCE: method involves material treatment with a solution containing nanostructured metal or oxide particles at a temperature of 20±5°C, and subsequent drying. The nonwoven material is subjected to ultrasonic pre-treatment to activate the surface and further processing by immersing or spraying a solution containing previously prepared nanoscale colloidal particles from metals or oxides at a concentration of 0.1-5% by material weight, followed by material drying at a temperature of 60 to 100°C to permanent weight.

EFFECT: invention allows to simplify the technology of preparation of the material with the required antibacterial characteristics, to increase strength and uniformity of nanoparticles fixation on the surface and in the material structure, which is especially necessary for development of membrane carriers sets for biological material transportation in veterinary laboratory diagnostics and epizootic monitoring, as dry stains applied to the carrier.

6 cl, 4 dwg, 1 tbl, 2 ex

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