CN103628104B - The optical fiber of optical fiber surface method for metallising, surface metalation and application thereof - Google Patents
The optical fiber of optical fiber surface method for metallising, surface metalation and application thereof Download PDFInfo
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- CN103628104B CN103628104B CN201310626267.7A CN201310626267A CN103628104B CN 103628104 B CN103628104 B CN 103628104B CN 201310626267 A CN201310626267 A CN 201310626267A CN 103628104 B CN103628104 B CN 103628104B
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Abstract
The invention relates to a kind of optical fiber surface method for metallising, the optical fiber of surface metalation and application thereof, described method comprises: immersed by optical fiber in the titanium chloride aqueous solution of 0.09-0.15g/L, thermostatically heating to 45-55 DEG C, insulation reaction 0.5-1.5h, take out described optical fiber, dry; Immersed in the tin chloride aqueous solution of 19-25g/L by the described optical fiber of drying, thermostatically heating is to 65-75 DEG C, and insulation reaction 5-15min, takes out described optical fiber, cleaning post-drying; Optical fiber above-mentioned steps obtained immerses in the first plating solution, at 75-85 DEG C, react 1-3min, takes out, immerse in the second plating solution, be react at least 7min under the microwave radiation of 1.5-2.0GHz in frequency, temperature of reaction is 45-55 DEG C, obtains the optical fiber of surface metalation.Optical fiber surface method for metallising provided by the invention make use of metal ion and deposits the constant speed of fiber, by the control to plating conditions, according to the plating speed difference of quick forming core and fine and close forming core, make metallic coating need not carry out roughening treatment and can grow nucleation, thus avoid the matrix that the plating of traditional alligatoring forming core brings and damage.
Description
Technical field
The present invention relates to technical field of optical fiber, particularly relate to the optical fiber of a kind of method for metallising not damaging optical fiber surface and the surface metalation prepared by the method.
Background technology
New Application Areas requires that photoconductive fiber has preferably resistance to abrasion, higher physical strength, comparatively small curvature radius can be carried out bend, novel integrated electro-optical system due to live width narrower, optical fiber repeatedly need wear in the temperature field that gradient is larger around, therefore the thermal stresses solving fiber generation is also needed, to avoid fibercuts.
Conventional optical fiber because of its surface plastic materials protection big envelope thickness large, and wear resistance, thermostability and conductivity are poor, are not suitable for the communications field that live width is narrower, thermograde is larger.Usually carry out compact metal process at optical fiber surface and solve the problems referred to above.The increase of metallic coating is conducive to the physical strength of reinforcing fibre, strengthens its wear resistance, and high-thermal conductive metal is conducive to improving the thermal stresses impact of fiber under high-temperature gradient simultaneously.
Due to quartz, glass-like materials fiber quality is hard, specific surface area is larger, be difficult to metallizing coating, the method of compact metal process is carried out mainly by soaking filamentary material in strong acid-base at such optical fiber surface, make its microcosmic surface be covered with groove, hole, utilize groove, the high surface energy of hole class defect carrys out metal refining.
The fiber carrying out surface metalation by aforesaid method is generally used for electromagnetic shielding etc. to glass surface without the field of being strict with, and but cannot be used for optical commucication, especially integration module photoelectric communication field.
Summary of the invention
In order to solve the problem of prior art, on the one hand, the invention provides a kind of optical fiber surface method for metallising, comprise the following steps:
(1) immerse in the titanium chloride aqueous solution of 0.09-0.15g/L by optical fiber, thermostatically heating is to 45-55 DEG C, and insulation reaction 0.5-1.5h, takes out described optical fiber, dries; Directly dry after taking out described optical fiber in this step, do not clean.
The main component of optical fiber is silicon-dioxide, it is inorganic non-metallic, the associativity of common metal particle and inorganic non-metallic is poor, and titanium belongs to oxytropism metal, itself and non-metallic material associativity are better, by forming one deck titanium particle layer at optical fiber surface, be conducive to the attachment of other metallicss in subsequent step.
(2) immersed in the tin chloride aqueous solution of 19-25g/L by the described optical fiber of drying, thermostatically heating is to 65-75 DEG C, and insulation reaction 5-15min, takes out described optical fiber, cleaning post-drying;
Optical fiber surface is made to be attached with appropriate tin by this step, for subsequent technique provides the rational reductive agent of reduction intensity.
(3) optical fiber that above-mentioned steps obtains is immersed in the first plating solution, at 75-85 DEG C, react 1-3min, take out, immerse in the second plating solution, be react at least 7min under the microwave radiation of 1.5-2.0GHz in frequency, temperature of reaction is 45-55 DEG C, obtains the optical fiber of surface metalation;
Wherein:
The first described plating solution is made up of following weight part material: the anhydrous sodium hypophosphite of 10-15 part, 28-33 part anhydrous nickel sulfate, 8-12 part trisodium citrate, 10-14 part anhydrous sodium acetate and 1000 weight parts waters; The second described plating solution is made up of following weight part material: the anhydrous sulfate of the anhydrous sodium hypophosphite of 13-18 part, 38-43 part plating metal, 8-12 part trisodium citrate, 10-14 part anhydrous sodium acetate and 1000 weight parts waters; The present invention is by the plating solution of use two kinds of different concns, and control metal nucleation rate by the cooperation of two concentration, the first plating solution forms metal nucleation center fast, and the second plating solution realizes coating around nucleating center densification growth.Preferably, the first described electroplate liquid is made up of following weight part material: 12 parts of anhydrous sodium hypophosphites, 30 parts of anhydrous nickel sulfates, 10 parts of trisodium citrates, 12 parts of anhydrous sodium acetates and 1000 weight parts waters; The second described electroplate liquid is made up of following weight part material: the anhydrous sulfate of 15 parts of anhydrous sodium hypophosphites, 40 parts of plating metals, 10 parts of trisodium citrates, 12 parts of anhydrous sodium acetates and 1000 weight parts waters.In the plating solution of this concentration, when reacting at 50 DEG C under the microwave radiation in frequency being 1.8GHz, the formation speed of metallic coating is about 0.5 [mu, and speed of reaction is moderate.
Preferably, described optical fiber adopts silica fiber or S-glass fibre, and the diameter of described silica fiber or S-glass fibre is 6-100 micron.Silica fiber or S-glass fibre have higher fusing point and chemical stability, monofilament Young's modulus 4000-5000MPa, Young's modulus is 85-93GPa, more than 20% is improved than E-glass fiber single filament intensity raising more than 30%, Young's modulus, after plating metallic diaphragm, overall mechanical property is better than the fiber that other has identical plated film.
Preferably, described plating metal is copper or nickel.Specifically select which kind of metal can require to determine according to the degree of crook of optical fiber, when requiring higher to the crooking ability of optical fiber, preferable alloy copper, the preferable alloy nickel when the crooking ability of optical fiber requires lower.
Preferably, also comprise before step (1): deionized water optical fiber being placed in 65-75 DEG C, ultrasonic vibration cleans at least 20min, vacuum-drying.Effectively can be removed the impurity of optical fiber surface by this step, be conducive to metal ion and adhere at optical fiber surface.
Preferably, the described oven dry in step (1), carries out at 95-105 DEG C.Ensure that titanium ion does not destroy optical fiber cladding at such a temperature, avoid exchange of substance that is extraneous and optical fiber cladding.
Preferably, the described cleaning, drying in step (2), comprising: described optical fiber is statically placed in 4-7min in deionized water at normal temperature, the metallic tin that cleaning removing optical fiber surface is unnecessary, avoids it to be free in follow-up plating solution and pollutes plating solution, take out and dry.
On the other hand, the invention provides a kind of optical fiber of the surface metalation prepared by aforesaid method.
Another aspect, the invention provides the application of optical fiber in optical communications field of above-mentioned surface metalation.
By technique scheme, a kind of optical fiber surface method for metallising of the present invention at least has following advantages:
Optical fiber surface method for metallising provided by the invention make use of metal ion and deposits the constant speed of fiber, by the control to plating conditions, according to the plating speed difference of quick forming core and fine and close forming core, make metallic coating need not carry out roughening treatment and can grow nucleation, thus avoid the matrix that the plating of traditional alligatoring forming core brings and damage, by the rational reduction intensity of solution system, utilizing microwave exposure to make metallic charged particles repeatedly clash into fiber, can become seal the alloyed metal coating wrapped up in ringwise at fiber surface uniform deposition without the need to destroying fiber microcosmic surface.It is metalized coated that the embodiment of the present invention provides, meet the requirement strengthening photoconductive fiber wear resistance, improve heat conduction efficiency, this coating has good high-temperature oxidation, the high temperature oxidation resisting characteristic of cupronickel is more excellent, can reach oxidizing temperature under atmospheric environment, up to 550 DEG C, descends oxidizing temperature up to 720 DEG C under rare gas element or vacuum environment; Under domestic electromagnetic frequency, the skin depth of microwave is within 1.5 microns, and the optical fiber of surface metalation that therefore embodiment of the present invention provides is applicable to the field such as Electromgnetic seat, shielding.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technique means of the present invention, and can be implemented according to the content of specification sheets, be described in detail as follows below with preferred embodiment of the present invention.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but not as a limitation of the invention.
Embodiment 1
Plating pre-treatment:
(1) optical fiber is placed in the deionized water of 70 DEG C, ultrasonic vibration cleaning 30min, vacuum-drying.
(2) optical fiber after step (1) being processed immerses in the titanium chloride aqueous solution of 0.13g/L, thermostatically heating to 50 DEG C, and insulation reaction 1h, takes out described optical fiber, 100 DEG C of oven dry;
(3) immerse in the tin chloride aqueous solution of 20g/L by the described optical fiber of drying, thermostatically heating to 70 DEG C, insulation reaction 10min, takes out described optical fiber, is statically placed in deionized water at normal temperature to take out after 5min to dry;
Plating:
(4) optical fiber that above-mentioned steps (3) obtains is immersed in the first plating solution, at 75-85 DEG C, react 1-3min, take out;
(5) immerse in the second plating solution, be react 10min under the microwave radiation of 1.8GHz in frequency, temperature of reaction is 50 DEG C, obtains the optical fiber of surface metalation;
In this step, the first described plating solution is the mixed aqueous solution of sodium hypophosphite, single nickel salt, trisodium citrate and sodium acetate, wherein NaH
2pO
2concentration be 12 grams per liters, NiSO
4concentration be 30 grams per liters, the concentration of trisodium citrate is 10 grams per liters, the concentration of anhydrous sodium acetate is 12 grams per liters; The second described plating solution is the mixed aqueous solution of sodium hypophosphite, copper sulfate, trisodium citrate and sodium acetate, wherein NaH
2pO
2concentration be 15 grams per liters, CuSO
4concentration be 40 grams per liters, the concentration of trisodium citrate is 10 grams per liters, the concentration of anhydrous sodium acetate is 12 grams per liters.Under this reaction conditions, metal level generates with the speed of 0.2 [mu, can pass through adjusting reaction time, changes metal layer thickness.
Embodiment 2
Plating pre-treatment:
(1) optical fiber is placed in the deionized water of 65 DEG C, ultrasonic vibration cleaning 40min, vacuum-drying.
(2) optical fiber after step (1) being processed immerses in the titanium chloride aqueous solution of 0.13g/L, thermostatically heating to 45 DEG C, and insulation reaction 1.5h, takes out described optical fiber, 95 DEG C of oven dry;
(3) immerse in the tin chloride aqueous solution of 20g/L by the described optical fiber of drying, thermostatically heating to 65 DEG C, insulation reaction 15min, takes out described optical fiber, is statically placed in deionized water at normal temperature to take out after 4min to dry;
Plating:
(4) optical fiber that above-mentioned steps (3) obtains is immersed in the first plating solution, at 75 DEG C, react 3min, take out;
(5) immerse in the second plating solution, be react 7min under the microwave radiation of 2.0GHz in frequency, temperature of reaction is 55 DEG C, obtains the optical fiber of surface metalation;
In this step, the first described plating solution is the mixed aqueous solution of sodium hypophosphite, single nickel salt, trisodium citrate and sodium acetate, wherein NaH
2pO
2concentration be 12 grams per liters, NiSO
4concentration be 30 grams per liters, the concentration of trisodium citrate is 10 grams per liters, the concentration of anhydrous sodium acetate is 12 grams per liters; The second described plating solution is the mixed aqueous solution of sodium hypophosphite, copper sulfate, trisodium citrate and sodium acetate, wherein NaH
2pO
2concentration be 15 grams per liters, CuSO
4concentration be 40 grams per liters, the concentration of trisodium citrate is 10 grams per liters, the concentration of anhydrous sodium acetate is 12 grams per liters.
Embodiment 3
Plating pre-treatment:
(1) optical fiber is placed in the deionized water of 75 DEG C, ultrasonic vibration cleaning 20min, vacuum-drying.
(2) optical fiber after step (1) being processed immerses in the titanium chloride aqueous solution of 0.13g/L, thermostatically heating to 55 DEG C, and insulation reaction 0.5h, takes out described optical fiber, 105 DEG C of oven dry;
(3) immerse in the tin chloride aqueous solution of 20g/L by the described optical fiber of drying, thermostatically heating to 75 DEG C, insulation reaction 5min, takes out described optical fiber, is statically placed in deionized water at normal temperature to take out after 7min to dry;
Plating:
(4) optical fiber that above-mentioned steps (3) obtains is immersed in the first plating solution, at 85 DEG C, react 1min, take out;
(5) immerse in the second plating solution, be react 8min under the microwave radiation of 1.5GHz in frequency, temperature of reaction is 55 DEG C, obtains the optical fiber of surface metalation;
In this step, the first described plating solution is the mixed aqueous solution of sodium hypophosphite, single nickel salt, trisodium citrate and sodium acetate, wherein NaH
2pO
2concentration be 12 grams per liters, NiSO
4concentration be 30 grams per liters, the concentration of trisodium citrate is 10 grams per liters, the concentration of anhydrous sodium acetate is 12 grams per liters; The second described plating solution is the mixed aqueous solution of sodium hypophosphite, copper sulfate, trisodium citrate and sodium acetate, wherein NaH
2pO
2concentration be 15 grams per liters, CuSO
4concentration be 40 grams per liters, the concentration of trisodium citrate is 10 grams per liters, the concentration of anhydrous sodium acetate is 12 grams per liters.
Embodiment 4
Plating pre-treatment and plating technology condition identical with embodiment 1, unlike:
In step (2), the concentration of titanium chloride aqueous solution is 0.09g/L;
In step (3), the concentration of the tin chloride aqueous solution is 19g/L;
NaH in step (4)
2pO
2concentration be 10 grams per liters, NiSO
4concentration be 28 grams per liters, the concentration of trisodium citrate is 8 grams per liters, the concentration of anhydrous sodium acetate is 10 grams per liters;
NaH in step (5)
2pO
2concentration be 13 grams per liters, CuSO
4concentration be 38 grams per liters, the concentration of trisodium citrate is 8 grams per liters, the concentration of anhydrous sodium acetate is 10 grams per liters.
Embodiment 5
Plating pre-treatment and plating technology condition identical with embodiment 1, unlike:
In step (2), the concentration of titanium chloride aqueous solution is 0.15g/L;
In step (3), the concentration of the tin chloride aqueous solution is 25g/L;
NaH in step (4)
2pO
2concentration be 15 grams per liters, NiSO
4concentration be 33 grams per liters, the concentration of trisodium citrate is 12 grams per liters, the concentration of anhydrous sodium acetate is 14 grams per liters;
NaH in step (5)
2pO
2concentration be 18 grams per liters, CuSO
4concentration be 43 grams per liters, the concentration of trisodium citrate is 12 grams per liters, the concentration of anhydrous sodium acetate is 14 grams per liters.
Embodiment 6
Plating pre-treatment and plating technology condition identical with embodiment 1, uniquely unlike: step uses NiSO in (5)
4substitute CuSO
4.
The optical fiber property of the surface metalation that embodiment 1-6 provides is see table one.Wherein, oxidizing temperature is determined being heated to the direct current ratio resistance (ohm/cm) before and after certain temperature by measuring fiber, changes, then think that fiber is oxidized if resistance be the order of magnitude.
The performance perameter table of the optical fiber of table one surface metalation
It is metalized coated for alloy coat that the embodiment of the present invention provides, meet the requirement strengthening photoconductive fiber wear resistance, improve heat conduction efficiency, this coating has good high-temperature oxidation, the high temperature oxidation resisting characteristic of cupronickel is more excellent, can reach oxidizing temperature under atmospheric environment, up to 550 DEG C, descends oxidizing temperature up to 720 DEG C under rare gas element or vacuum environment; Under domestic electromagnetic frequency, the skin depth of microwave is within 1.5 microns, therefore the optical fiber of surface metalation that the embodiment of the present invention provides is applicable to the field such as Electromgnetic seat, shielding, simultaneously, the optical fiber surface of the surface metalation provided due to the embodiment of the present invention is smooth, therefore optical commucication is applicable to, especially integration module photoelectric communication field.
Processing method of the present invention, had both maintained convenience and the cost requirement of traditional technology, had effectively maintained again the structure of photoconductive fiber itself, material integrity, had good engineering and economic benefit prospect.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (10)
1. an optical fiber surface method for metallising, is characterized in that, comprises the following steps:
(1) immerse in the titanium chloride aqueous solution of 0.09-0.15g/L by optical fiber, thermostatically heating is to 45-55 DEG C, and insulation reaction 0.5-1.5h, takes out described optical fiber, dries;
(2) immersed in the tin protochloride aqueous solution of 19-25g/L by the described optical fiber of drying, thermostatically heating is to 65-75 DEG C, and insulation reaction 5-15min, takes out described optical fiber, cleaning post-drying;
(3) optical fiber that above-mentioned steps obtains is immersed in the first plating solution, at 75-85 DEG C, react 1-3min, take out, immerse in the second plating solution, be react at least 7min under the microwave radiation of 1.5-2.0GHz in frequency, temperature of reaction is 45-55 DEG C, obtains the optical fiber of surface metalation;
Wherein:
The first described plating solution is made up of following weight part material: the anhydrous sodium hypophosphite of 10-15 part, 28-33 part anhydrous nickel sulfate, 8-12 part trisodium citrate, 10-14 part anhydrous sodium acetate and 1000 weight parts waters;
The second described plating solution is made up of following weight part material: the anhydrous sulfate of the anhydrous sodium hypophosphite of 13-18 part, 38-43 part plating metal, 8-12 part trisodium citrate, 10-14 part anhydrous sodium acetate and 1000 weight parts waters.
2. optical fiber surface method for metallising according to claim 1, is characterized in that:
Described optical fiber adopts silica fiber or S-glass fibre, and the diameter of described silica fiber or S-glass fibre is 6-100 micron.
3. optical fiber surface method for metallising according to claim 1, is characterized in that:
Described plating metal is copper or nickel.
4. optical fiber surface method for metallising according to claim 1, is characterized in that:
The first described electroplate liquid is made up of following weight part material: 12 parts of anhydrous sodium hypophosphites, 30 parts of anhydrous nickel sulfates, 10 parts of trisodium citrates, 12 parts of anhydrous sodium acetates and 1000 weight parts waters.
5. optical fiber surface method for metallising according to claim 4, is characterized in that:
The second described electroplate liquid is made up of following weight part material: the anhydrous sulfate of 15 parts of anhydrous sodium hypophosphites, 40 parts of plating metals, 10 parts of trisodium citrates, 12 parts of anhydrous sodium acetates and 1000 weight parts waters.
6. the optical fiber surface method for metallising according to any one of claim 1-5, is characterized in that, also comprises before step (1):
Optical fiber is placed in the deionized water of 65-75 DEG C, ultrasonic vibration cleans at least 20min, vacuum-drying.
7. the optical fiber surface method for metallising according to any one of claim 1-5, is characterized in that, the described oven dry in step (1), carries out at 95-105 DEG C.
8. the optical fiber surface method for metallising according to any one of claim 1-5, is characterized in that, the described cleaning, drying in step (2), comprising:
Described optical fiber is statically placed in 4-7min in deionized water at normal temperature, takes out and dry.
9. the optical fiber of the surface metalation prepared by the method described in any one of claim 1-8.
10. the application of optical fiber in optical communications field of surface metalation according to claim 9.
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| CN105250073B (en) * | 2015-11-12 | 2016-06-29 | 张开银 | A kind of conduction optical fiber bioelectrode being provided with multiple coat of metal and preparation method thereof |
| CN108363140B (en) * | 2018-04-02 | 2019-11-15 | 武汉虹拓新技术有限责任公司 | A kind of amplifying fiber resistant to high temperature |
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| CN1790059A (en) * | 2005-12-20 | 2006-06-21 | 武汉理工大学 | Wet chemical metallizing process for quartz optical fiber grating surface |
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| CN1790059A (en) * | 2005-12-20 | 2006-06-21 | 武汉理工大学 | Wet chemical metallizing process for quartz optical fiber grating surface |
Non-Patent Citations (3)
| Title |
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| A plating method for metal coating of f iber Bragg grating;Yulong Li et al;《Chinese Optical Letters》;20090210;第7卷(第2期);第115-117页 * |
| 光纤光栅金属化工艺及特性研究;姚文历等;《光电技术应用》;20121231;第27卷(第6期);第46-54页 * |
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