CN103628104A - Method for surface metallization of optical fiber, surface-metallized optical fiber and application thereof - Google Patents
Method for surface metallization of optical fiber, surface-metallized optical fiber and application thereof Download PDFInfo
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- CN103628104A CN103628104A CN201310626267.7A CN201310626267A CN103628104A CN 103628104 A CN103628104 A CN 103628104A CN 201310626267 A CN201310626267 A CN 201310626267A CN 103628104 A CN103628104 A CN 103628104A
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Abstract
The invention relates to a method for surface metallization of an optical fiber, a surface-metallized optical fiber and an application thereof. The method comprises the following steps: soaking the optical fiber into a 0.09-0.15g/L titanium chloride aqueous solution, performing constant-temperature heating until the temperature is 45-55 DEG C, performing thermal reaction for 0.5-1.5 hours, taking the optical fiber out, and drying the optical fiber; soaking the dried optical fiber in a 19-25g/L tin chloride aqueous solution, performing constant-temperature heating until the temperature is 65-75 DEG C, performing thermal reaction for 5-15 minutes, taking the optical fiber out, and cleaning and drying the optical fiber; soaking the optical fiber obtained by the previous step into a first plating solution, reacting for 1-3 minutes at 75-85 DEG C, taking the optical fiber out, soaking the optical fiber into a second plating solution, and reacting for at least 7 minutes at a reaction temperature of 45-55 DEG C under the radiation of microwaves of which the frequency is 1.5-2.0GHz to obtain the surface-metallized optical fiber. According to the method for surface metallization of the optical fiber, the constant deposition of metal ions on fibers is used, and a metal coating can grow into a core without roughening according to plating speed differences of a quick core and a compact core by controlling the plating condition, so that basic damages caused by the conventional roughening core formation plating are avoided.
Description
Technical field
The present invention relates to optical fiber technology field, particularly relate to a kind of optical fiber of the surface metalation that does not damage the method for metallising of optical fiber surface and prepare by the method.
Background technology
New Application Areas requires photoconductive fiber to have resistance to abrasion preferably, higher physical strength, can carry out crooked compared with small curvature radius, novel integrated electro-optical system is because live width is narrower, optical fiber need in the larger temperature field of gradient, repeatedly wear around, therefore also need to solve the thermal stresses that fiber produces, to avoid fibercuts.
Conventional light guides fiber because of its surperficial plastics 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.Conventionally at optical fiber surface, carry out compact metalization processing 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 improve the thermal stresses impact of fiber under high-temperature gradient simultaneously.
Due to quartzy, glass-like materials fiber quality is hard, specific surface area is larger, be difficult to metallizing coating, the method of carrying out compact metal processing at such optical fiber surface is mainly by soak filamentary material in strong acid-base, make its microcosmic surface be covered with groove, hole, utilize the high surface energy of groove, hole class defect to carry out metal refining.
The fiber that carries out surface metalation by aforesaid method be generally used for electromagnetic shielding etc. to glass surface without the field of being strict with, but cannot be for optical commucication, integration module photoelectric communication field especially.
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) optical fiber is immersed in the titanium chloride aqueous solution of 0.09-0.15g/L, thermostatically heating is to 45-55 ℃, and insulation reaction 0.5-1.5h, takes out described optical fiber, dries; After taking out described optical fiber in this step, directly dry, 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 form one deck titanium particle layer at optical fiber surface, be conducive to adhering to of other metallicss in subsequent step.
(2) the described optical fiber of drying is immersed in the tin chloride aqueous solution of 19-25g/L, thermostatically heating is to 65-75 ℃, and insulation reaction 5-15min, takes out described optical fiber, cleans post-drying;
By this step, make optical fiber surface be attached with appropriate tin, for subsequent technique provides reduction intensity rational reductive agent.
(3) optical fiber above-mentioned steps being obtained immerses in the first plating solution, at 75-85 ℃, reacts 1-3min, takes out, immerse in the second plating solution, under the microwave radiation that is 1.5-2.0GHz in frequency, react at least 7min, temperature of reaction is 45-55 ℃, obtains the optical fiber of surface metalation;
Wherein:
The first described plating solution is comprised 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 comprised 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, by using the plating solution of two kinds of different concns, controls metal nucleation rate by the cooperation of two concentration, and the first plating solution forms metal nucleation centre fast, and the second plating solution is realized coating fine and close growth around nucleating center.Preferably, the first described electroplate liquid is comprised 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 comprised 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, reaction at 50 ℃ under the microwave radiation that is 1.8GHz in frequency, the formation speed of metallic coating is about 0.5 micro-m/min, 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, than E-glass fiber single filament intensity improve more than 30%, Young's modulus improves more than 20%, after plating metallic diaphragm, whole mechanical property is better than other fiber with identical plated film.
Preferably, described plating metal is copper or nickel.Specifically select which kind of metal can be according to the degree of crook of optical fiber is required to determine, when the crooking ability of optical fiber is had relatively high expectations, preferable alloy copper, when the crooking ability of optical fiber requires preferable alloy nickel when lower.
Preferably, step (1) also comprises before: optical fiber is placed in to the deionized water of 65-75 ℃, at least 20min, vacuum-drying are cleaned in ultrasonic concussion.The impurity that can effectively remove optical fiber surface by this step, is conducive to metal ion and adheres at optical fiber surface.
Preferably, the described oven dry in step (1) is carried out at 95-105 ℃.At this temperature, guaranteed that titanium ion does not destroy optical fiber cladding, avoided exchange of substance extraneous and optical fiber cladding.
Preferably, the described cleaning, drying in step (2), comprising: described optical fiber is statically placed in to 4-7min in deionized water at normal temperature, cleans and remove the unnecessary metallic tin of optical fiber surface, avoid it to be free in follow-up plating solution and pollute plating solution, take out and dry.
On the other hand, the invention provides a kind of optical fiber of the surface metalation of being prepared by aforesaid method.
Another aspect, the application of the optical fiber that the invention provides above-mentioned surface metalation in optical communications field.
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 has utilized the constant speed deposition of metal ion to fiber, by the control to plating condition, according to the plating speed difference of quick forming core and fine and close forming core, make metallic coating needn't carry out the roughening treatment nucleation of can growing, thereby avoided the matrix that the plating of traditional alligatoring forming core brings to damage, by the rational reduction intensity of solution system, utilize microwave exposure to make metal charged particle repeatedly clash into fiber, without destroying fiber microcosmic surface, can become the alloyed metal coating that envelope is wrapped up in ringwise at fiber surface uniform deposition.It is metalized coated that the embodiment of the present invention provides, meet the requirement that strengthens photoconductive fiber wear resistance, improves 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 ℃, descends oxidizing temperature up to 720 ℃ under rare gas element or vacuum environment; Under domestic electromagnetic frequency, the skin depth of microwave is in 1.5 microns, so the optical fiber of the surface metalation that provides of the embodiment of the present invention is applicable to the fields 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, below with preferred embodiment of the present invention, is described in detail as follows.
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 to the deionized water of 70 ℃, 30min, vacuum-drying are cleaned in ultrasonic concussion.
(2) optical fiber after step (1) processing is immersed in the titanium chloride aqueous solution of 0.13g/L, thermostatically heating to 50 ℃, insulation reaction 1h, takes out described optical fiber, 100 ℃ of oven dry;
(3) the described optical fiber of drying is immersed in the tin chloride aqueous solution of 20g/L, thermostatically heating to 70 ℃, insulation reaction 10min, takes out described optical fiber, is statically placed in deionized water at normal temperature and takes out and dry after 5min;
Plating:
(4) optical fiber above-mentioned steps (3) being obtained immerses in the first plating solution, at 75-85 ℃, reacts 1-3min, takes out;
(5) immerse in the second plating solution, under the microwave radiation that is 1.8GHz, react 10min in frequency, temperature of reaction is 50 ℃, 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 that the concentration of 30 grams per liters, trisodium citrate is that the concentration of 10 grams per liters, 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 that the concentration of 40 grams per liters, trisodium citrate is that the concentration of 10 grams per liters, anhydrous sodium acetate is 12 grams per liters.Under this reaction conditions, metal level generates with the speed of 0.2 micro-m/min, can pass through adjusting reaction time, changes metal layer thickness.
Embodiment 2
Plating pre-treatment:
(1) optical fiber is placed in to the deionized water of 65 ℃, 40min, vacuum-drying are cleaned in ultrasonic concussion.
(2) optical fiber after step (1) processing is immersed in the titanium chloride aqueous solution of 0.13g/L, thermostatically heating to 45 ℃, insulation reaction 1.5h, takes out described optical fiber, 95 ℃ of oven dry;
(3) the described optical fiber of drying is immersed in the tin chloride aqueous solution of 20g/L, thermostatically heating to 65 ℃, insulation reaction 15min, takes out described optical fiber, is statically placed in deionized water at normal temperature and takes out and dry after 4min;
Plating:
(4) optical fiber above-mentioned steps (3) being obtained immerses in the first plating solution, at 75 ℃, reacts 3min, takes out;
(5) immerse in the second plating solution, under the microwave radiation that is 2.0GHz, react 7min in frequency, temperature of reaction is 55 ℃, 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 that the concentration of 30 grams per liters, trisodium citrate is that the concentration of 10 grams per liters, 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 that the concentration of 40 grams per liters, trisodium citrate is that the concentration of 10 grams per liters, anhydrous sodium acetate is 12 grams per liters.
Embodiment 3
Plating pre-treatment:
(1) optical fiber is placed in to the deionized water of 75 ℃, 20min, vacuum-drying are cleaned in ultrasonic concussion.
(2) optical fiber after step (1) processing is immersed in the titanium chloride aqueous solution of 0.13g/L, thermostatically heating to 55 ℃, insulation reaction 0.5h, takes out described optical fiber, 105 ℃ of oven dry;
(3) the described optical fiber of drying is immersed in the tin chloride aqueous solution of 20g/L, thermostatically heating to 75 ℃, insulation reaction 5min, takes out described optical fiber, is statically placed in deionized water at normal temperature and takes out and dry after 7min;
Plating:
(4) optical fiber above-mentioned steps (3) being obtained immerses in the first plating solution, at 85 ℃, reacts 1min, takes out;
(5) immerse in the second plating solution, under the microwave radiation that is 1.5GHz, react 8min in frequency, temperature of reaction is 55 ℃, 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 that the concentration of 30 grams per liters, trisodium citrate is that the concentration of 10 grams per liters, 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 that the concentration of 40 grams per liters, trisodium citrate is that the concentration of 10 grams per liters, anhydrous sodium acetate is 12 grams per liters.
Embodiment 4
Plating pre-treatment and plating technology condition are identical with embodiment 1, different:
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 that the concentration of 28 grams per liters, trisodium citrate is that the concentration of 8 grams per liters, anhydrous sodium acetate is 10 grams per liters;
NaH in step (5)
2pO
2concentration be 13 grams per liters, CuSO
4concentration be that the concentration of 38 grams per liters, trisodium citrate is that the concentration of 8 grams per liters, anhydrous sodium acetate is 10 grams per liters.
Embodiment 5
Plating pre-treatment and plating technology condition are identical with embodiment 1, different:
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 that the concentration of 33 grams per liters, trisodium citrate is that the concentration of 12 grams per liters, anhydrous sodium acetate is 14 grams per liters;
NaH in step (5)
2pO
2concentration be 18 grams per liters, CuSO
4concentration be that the concentration of 43 grams per liters, trisodium citrate is that the concentration of 12 grams per liters, anhydrous sodium acetate is 14 grams per liters.
Embodiment 6
Plating pre-treatment and plating technology condition are identical with embodiment 1, unique different: step is used NiSO in (5)
4substitute CuSO
4.
The optical fiber property of the surface metalation that embodiment 1-6 provides is referring to table one.Wherein, oxidizing temperature is determined than resistance (ohm/cm) at the direct current that is heated to certain temperature front and back by measuring fiber, if resistance is the order of magnitude, changes, and thinks that fiber is oxidized.
The performance perameter table of the optical fiber of table one surface metalation
It is metalized coated that the embodiment of the present invention provides is alloy coat, meet the requirement that strengthens photoconductive fiber wear resistance, improves 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 ℃, descends oxidizing temperature up to 720 ℃ under rare gas element or vacuum environment; Under domestic electromagnetic frequency, the skin depth of microwave is in 1.5 microns, the optical fiber of the surface metalation that therefore embodiment of the present invention provides is applicable to the fields such as Electromgnetic seat, shielding, simultaneously, the optical fiber surface of the surface metalation providing due to the embodiment of the present invention is smooth, therefore be applicable to optical commucication, especially integration module photoelectric communication field.
Processing method of the present invention, had both kept convenience and the cost requirement of traditional technology, had effectively maintained again structure, the material integrity of photoconductive fiber itself, had good engineering and economic benefit prospect.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, although the present invention discloses as above with preferred embodiment, yet not in order to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, when can utilizing the technology contents of above-mentioned announcement to make a little change or being modified to the equivalent embodiment of equivalent variations, in every case be the content that does not depart from technical solution of the present invention, any simple modification of above embodiment being done according to technical spirit of the present invention, 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) optical fiber is immersed in the titanium chloride aqueous solution of 0.09-0.15g/L, thermostatically heating is to 45-55 ℃, and insulation reaction 0.5-1.5h, takes out described optical fiber, dries;
(2) the described optical fiber of drying is immersed in the tin chloride aqueous solution of 19-25g/L, thermostatically heating is to 65-75 ℃, and insulation reaction 5-15min, takes out described optical fiber, cleans post-drying;
(3) optical fiber above-mentioned steps being obtained immerses in the first plating solution, at 75-85 ℃, reacts 1-3min, takes out, immerse in the second plating solution, under the microwave radiation that is 1.5-2.0GHz in frequency, react at least 7min, temperature of reaction is 45-55 ℃, obtains the optical fiber of surface metalation;
Wherein:
The first described plating solution is comprised 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 comprised 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 comprised 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 comprised 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. according to the optical fiber surface method for metallising described in claim 1-5 any one, it is characterized in that, step (1) also comprises before:
Optical fiber is placed in to the deionized water of 65-75 ℃, at least 20min, vacuum-drying are cleaned in ultrasonic concussion.
7. according to the optical fiber surface method for metallising described in claim 1-5 any one, it is characterized in that, the described oven dry in step (1) is carried out at 95-105 ℃.
8. according to the optical fiber surface method for metallising described in claim 1-5 any one, it is characterized in that, the described cleaning, drying in step (2), comprising:
Described optical fiber is statically placed in to 4-7min in deionized water at normal temperature, takes out and dry.
9. the optical fiber of the surface metalation of being prepared by the method described in claim 1-8 any one.
10. the application of the optical fiber of surface metalation claimed in claim 9 in optical communications field.
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| CN201310626267.7A CN103628104B (en) | 2013-11-28 | 2013-11-28 | The optical fiber of optical fiber surface method for metallising, surface metalation and application thereof |
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| CN105250073A (en) * | 2015-11-12 | 2016-01-20 | 张开银 | Conductive optical fiber bioelectrode provided with multiple metal coatings and preparation method thereof |
| CN108363140A (en) * | 2018-04-02 | 2018-08-03 | 武汉虹拓新技术有限责任公司 | A kind of heat safe amplifying fiber |
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105250073A (en) * | 2015-11-12 | 2016-01-20 | 张开银 | Conductive optical fiber bioelectrode provided with multiple metal coatings and preparation method thereof |
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| CN108363140A (en) * | 2018-04-02 | 2018-08-03 | 武汉虹拓新技术有限责任公司 | A kind of heat safe amplifying fiber |
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