CN107620064A - A kind of fibre optical sensor metallization packaged method and technique - Google Patents
A kind of fibre optical sensor metallization packaged method and technique Download PDFInfo
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Abstract
The present invention is a kind of fibre optical sensor metallization packaged method and technique, (1) Pre-treatment before plating, cleans and is roughened optical fiber surface；(2) fiber grating is sensitized and activation process, makes its surface that there is certain catalytic activity；(3) chemical nickel plating, one layer of conductive, fine and close, uniform nickel-phosphorus alloy coating is deposited in optical fiber surface；(4) plating metal, controls electroplating time and magnitude of voltage, plating metal on the grating after chemical plating, customizes the shape specification of different matrix, obtains adapting to the metal coating grating of different condition according to the actual requirements.One aspect of the present invention effectively enhances the temperature characterisitic and pressure characteristic of grating, improves the measurement accuracy of sensor；On the other hand the features such as avoiding poor adhesive easy to aging, easy creep, corrosion resistance, shock resistance difference, the service life of fibre optical sensor is effectively extended.
Description
Technical field
The invention belongs to photoelectricity biology sensor field, more particularly to a kind of fibre optical sensor metallization packaged method and work
Skill.
Background technology
Fibre optical sensor has small volume, in light weight, precision is high, service life is long, anti-electromagnetic interference capability is strong, waterproof is prevented
The advantages that tide and intrinsic safety, it is widely used in the peace in the fields such as Geological Engineering, Structural Engineering, Tunnel Engineering, science of bridge building
In full monitoring.At present, fibre optical sensor is generally by the way of colloid encapsulation, but colloid has easy to aging, easy creep, corrosion resistant
The features such as losing ability, shock resistance difference, seriously limit shelf life and the measurement accuracy of fibre optical sensor.It is well known that
Part metals have the characteristic such as corrosion-resistant, high pressure resistant, high temperature resistant, use welding manner carry out fibre-optic sensor package be overcome with
The effective ways of upper problem, but the main component of optical fiber is silica, is nonmetallic materials, it is impossible to directly carry out welding envelope
Dress.Therefore, optical fiber surface is metallized, and then realizes the metallization packaged of fibre optical sensor, have important economic implications and
Practical value.
Silica fibre surface metalation has a variety of methods, is such as evaporated in vacuo plating method, sputtering method, melting painting plating method, chemical plating
Method, galvanoplastic etc..But due to unmanageable in operation, reason, the current various techniques such as raw material is special, processing cost is high
Remain respective deficiency and limitation.For this present situation, there is an urgent need to break through optical fiber metallization process key technology
Problem, to meet actual use demand.
Zhang Shengfeng on《Silica fibre surface metalation》Research：It is prepared for by chemical nickel plating+plating with mangneto
The nickel-cobalt alloy plating silica fibre of telescopicing performance.But during its chemical nickel plating, a large amount of hydrogen that separate out be present and cause solution ph to decline,
Active crystal is decomposed the problem of making bath stability difference.
The content of the invention
In order to overcome above-mentioned deficiency, the present invention proposes a kind of chemical plating with electroplating the optical fiber metallization packaged side being combined
Method and technique, one layer of even compact and the good coat of metal of adhesion have been obtained in optical fiber surface, enhance the toughness of grating with
High temperature resistant, corrosion resistance, to realize that the long-life packages of fibre optical sensor provide effective method.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of fibre optical sensor metallization packaged method, including：
Optical fiber is pre-processed, is sensitized, is activated, chemical nickel plating, plating metal, is produced；
The nickel liquid of the chemical nickel plating includes：Main salt nickel sulfate, reducing agent sodium hypophosphite, complexing agent 85wt% breast
Acid, buffer boric acid, stabilizer sodium fluoride, and ammoniacal liquor.
Present invention research is found：The hydrogen largely separated out when can prevent chemical nickel plating using 35g/L boric acid as buffer causes
Solution ph declines；Stabilizer 30g/L sodium fluorides are sheltered to active crystal, can effectively prevent plating solution selfdecomposition；Meanwhile
The pH value of buffer ammoniacal liquor adjustment plating solution is added in course of reaction, ensures the stability of plating solution.With this, chemistry of the invention ensure that
The stability of nickel-plating liquid, improve the stability, uniformity and compactness of coating.
Preferably, the electroplating solution of the plating metal includes：Pyrophosphoric acid, potassium pyrophosphate, the hydrate of sodium potassium tartrate tetrahydrate four
Thing, dipotassium hydrogen phosphate, phytic acid, vanillic aldehyde, copper-bath, and ammoniacal liquor.
Preferably, the pretreating process includes：Deprotect layer, cleaning, oil removing, cleaning, remove metal ion, cleaning,
Chemistry roughening, cleaning, heat treatment.
It is furthermore preferred that NaOH solution of the oil removing of the present invention using alkali lye 20wt%, compared to removing for acid deoiling liquid
Oily ability is strong, cheap.
It is furthermore preferred that the present invention removes the metal ion adhered in fiber preparation from dilute nitric acid solution, in order to avoid
The strong metal ion of some reproducibilities influences chemical nickel plating and plating metal process, improves the quality of coating.
Preferably, SnCl is selected in the sensitization of described optical fiber surface and activation2With Cu respectively as sensitizer and with catalysis
The metallic element of activity, using impregnation catalyst metal activation method, optical fiber surface is set to cover one layer of catalytic membrane.
Preferably, the plating metal, configures electroplate liquid in proportion, during specific electro-coppering, regulation pH value to 7 or so,
Temperature is 20 DEG C, electric current 0.5A/dm2Under conditions of, electroplate 20-30min.
Preferably, coarsening time control is in 3min or so, obtains that surface is smooth, covering is good, complete uniform plating
Layer.
Preferably, activation temperature control is at 30-40 DEG C, soak time 20min.
Preferably, the chemical nickel plating concretely comprises the following steps：First, the 85wt% lactic acid of measured amounts be added to from
Enveloping agent solution is mixed into sub- water, then weighs quantitative 30g/L nickel sulfates, 28g/L sodium hypophosphites, 35g/L boron respectively
Acid and 30g/L sodium chloride are added in enveloping agent solution, finally add ammoniacal liquor to adjust the pH value of plating solution；In 20-25 DEG C of bar
Under part, optical fiber is inserted into 5-10min in chemical nickel-plating liquid.
Preferably, the plating metal concretely comprises the following steps：The fiber grating that surface has nickel-phosphorus alloy coating is spent
Ionized water is cleaned and dried, and is then attached on negative electrode；Anode uses graphite electrode, first goes oil removing with 10wt% NaOH solution
It is dirty；Mass concentration 10wt% H is used again2SO4Solution neutralizes, and is then cleaned with distilled water, and under given technique, it is molten to be placed in plating
30min is electroplated in liquid.
It is furthermore preferred that the electroplating solution and electroplating technology that the present invention uses are as follows：
Copper electroplating solution is by 60g/L pyrophosphoric acids, 300g/L potassium pyrophosphate, the 40g/L hydrate of sodium potassium tartrate tetrahydrate four,
40g/L dipotassium hydrogen phosphates, 0.2g/L phytic acid, 0.1g/L vanillic aldehyde composition.In pH6.0-7.0,20 DEG C of temperature, electric current
0.5A/dm2Process conditions under, electroplate 20-30min, obtain the copper plating film of even compact.
Gold-plating solution is by 15-18g/L citric acids, 45g/L chlorauride, 35g/L potassium permanganate, 2g polishing agent groups
Into.In pH6.5-7.0,25 DEG C of temperature, electric current 0.6A/dm2Process conditions under, electroplate 30min, obtain the gold-plated of even compact
Film.
Electroplate zinc solution and 200mL electroplating solution is formed by 80g zinc sulfate, 6g boric acid, 2g polishing agents, 2g polishing agents.
Under 3V voltages, 25min is electroplated, obtains the zinc-plated film of even compact.
Present invention also offers fibre optical sensor prepared by any above method.
Beneficial effects of the present invention
(1) the optical fiber grating temperature characteristic by surface metalation processing is studied in the present invention, found due to gold
The thermal coefficient of expansion of category is larger, and metal coating grating serves temperature sensitizing effect, improves the temperature control of sensor；
To be tested by stress loading, it was demonstrated that the metallization packaged designed by the present invention has an impact to grating mechanical performance,
In stress loading to certain limit, strain transducer characteristic can keep the linearity and repeatability of height.
Meanwhile the fiber grating after metallization packaged is connect with adhesion without adhesiver realizes the integrated of FBG- metal composite structures, with
Conventional package mode is compared, and high temperature resistant, corrosion-resistant, measurement accuracy is high.
(2) plating metal on the basis of chemical nickel plating, avoid long-time chemical plating and thicken coating, cause coating not connect
The continuous phenomenon even to come off.It and this method is easy and effective, can be required according to different sensors, customize different basic configuration rule
Lattice, and the metal of different-thickness is plated according to the actual requirements.
(3) present invention carries out metallization packaged by the way of plating is combined using chemical plating to optical fiber, and technique is used
Raw material is easy to get, and operating process is simple, and cost is low；
(4) metallization packaged of grating sensor, support is provided to improve the life-span of sensor.
(5) preparation method of the present invention is simple, high sensitivity, practical, easy to spread.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not form the improper restriction to the application.
Fig. 1 is different voltages, different time electroplating effect comparison diagram；
Fig. 2, Fig. 3, Fig. 4 are respectively the SEM testing result figures of copper facing grating, gold-plated grating, zinc-plated grating；
Fig. 5 is metal coating grating temperature performance diagram；
Fig. 6 is strain-gauge test platform schematic diagram；
Fig. 7 is the emergent property curve map of metal coating grating；
Fig. 8 is the process chart of the present invention.
Embodiment
It is noted that described further below is all exemplary, it is intended to provides further instruction to the application.It is unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
A kind of fibre optical sensor metallization packaged method and technique, include following step.First, Pre-treatment before plating, go
Dirt, grease and oxide skin except optical fiber surface etc.；Then, further optical fiber surface is sensitized and activated, so that its
Surface has certain catalytic activity；Then, chemical nickel plating, on FBG surfaces, one layer of deposition has conductive power, smooth
Nickel-phosphorus alloy firm；Finally, plating metal, the grating after chemical plating is electroplated onto on sheet metal, by change electroplating time and
Voltage, obtain adapting to the metal coating grating of different condition.
The flow that described Pre-treatment before plating uses for：Deprotect layer-cleaning-oil removing-cleaning-removal metal from
Son-cleaning-chemical roughening-cleaning-heat treatment.
Described optical fiber surface sensitization and activation, specifically from SnCl2Lived with Cu respectively as sensitizer and with catalysis
Property metallic element, using leaching catalytic metal activation method, make optical fiber surface cover one layer of catalytic membrane.
The chemical nickel plating, determines the various components of chemical nickel-plating liquid, and this patent includes main salt nickel sulfate, reducing agent time Asia
Sodium phosphate, the lactic acid of complexing agent 85%, buffer boric acid, stabilizer sodium fluoride；Controlled during the course of the reaction by adding ammoniacal liquor
The volume of solution processed simultaneously adjusts bath pH value.
The plating metal, plating metal solution is configured in proportion.By taking electro-coppering as an example, solution ph is 7.0 or so, electricity
Pressure setting 3V, electroplating current 0.5A/dm2, electroplate 20-30 minutes.
Compared with traditional metallization encapsulates, the present invention plating metal, forms even compact on the basis of chemical nickel plating
Coating.The adhesive mode of FBG- metal composite structures is avoided, while improves fiber grating temperature sensor characteristic, emergent property,
It is corrosion-resistant, resistance to pressure, expand FBG use range.
The embodiment of the technique is as follows：
Step 1 optical fiber Pre-treatment before plating
(1-1) deprotects layer：
The method being combined using chemical immersion and mechanical stripping, is concretely comprised the following steps first to wait to divest by optical fiber and is partially disposed in
5-15min is soaked in the 98wt% concentrated sulfuric acid；Lightly protective layer is removed with optical fiber ablation scissors after taking-up, then uses alcohol
Cotton is gently wiped 4-6 times；Finally it is cleaned by ultrasonic 5min in deionized water；
(1-2) oil removing：
Optical fiber part to be plated is immersed in the NaOH solution that mass concentration is 20%, soaks 20min；Distinguish again after taking-up
It is placed in absolute ethyl alcohol and deionized water and is cleaned by ultrasonic 5-10min；
(1-3) removes metal ion：
Optical fiber 5-10min is soaked from dilute nitric acid solution, optical fiber is placed in deionized water after taking-up and cleaned with ultrasonic wave
3min, that is, complete the removal of the impurity such as metal and metal ion；
The roughening of (1-4) chemistry：
Using mixed acid, contain hydrofluoric acid or F-Strongly acidic solution weak corrosion 3min is carried out to quartzy FBG；
(1-5) is heat-treated：
Quartzy FBG after roughening is immersed in 10min in the water more than 100 DEG C, removes the moisture film of optical fiber surface.
Step 2 is sensitized and activation
Under the constant temperature that 30-40 DEG C of (2-1), optical fiber is immersed into the SnCl by 10g/L2Formed with 40ml/L hydrochloric acid
15min or so in sensitizing solution, is finally cleaned by ultrasonic 2min in deionized water；
(2-2) keeps sensitization constant temperature, by the activating solution that the optical fiber after sensitization is placed in copper chloride and hydrochloric acid configuration forms
Middle processing 20min.
Step 3 chemical nickel plating
(3-1) determines chemical nickel-plating liquid component, and the present invention is from nickel sulfate as main salt, and sodium hypophosphite is as reduction
Agent, 85wt% lactic acid is as complexing agent, and boric acid is as buffer, and sodium fluoride is as stabilizer；
(3-2) configures chemical nickel-plating liquid, and 85% lactic acid of measured amounts first, which is added in deionized water, is mixed into network
Mixture solution, quantitative nickel sulfate, sodium hypophosphite, boric acid and sodium fluoride are then weighed respectively and is added in enveloping agent solution,
Ammoniacal liquor is finally added to adjust the pH value of plating solution.
(3-3) inserts 5-10min in chemical nickel-plating liquid under conditions of 20-25 DEG C, by optical fiber.
Step 4 plating metal
By taking electro-coppering as an example, the fiber grating that surface is had to the nickel-phosphorus alloy of conductive power is cleaned and done with deionized water
It is dry, it is then attached on negative electrode.Anode uses graphite electrode, is first degreased with 10wt% NaOH solution, then use 10wt%
H2SO4Solution neutralizes, and is then cleaned with distilled water, under given technique, is placed in electroplating solution and electroplates 20-30min.
Further, described step (1-4) strictly controls coarsening time, if coarsening time is long, can cause optical fiber
Surface roughness is excessive.Palladium metal deposition is uneven, rough spot occurs, or even cause and come off.
Further, described step (3-3) adds ammoniacal liquor to adjust in real time when optical fiber is inserted and reacted in chemical nickel-plating liquid
The pH value of whole nickel-plating liquid, to ensure the stability of plating solution.
Further, the electroplating solution preparation method of the step 4, by 60g/L pyrophosphoric acids, 300g/L potassium pyrophosphate,
The 40g/L hydrate of sodium potassium tartrate tetrahydrate four, 40g/L dipotassium hydrogen phosphates, 0.2g/L phytic acid, 0.1g/L vanillic aldehyde, slowly
Add in copper-bath, be stirred continuously, until there is white precipitate generation, solution is in sky blue.If pH value is relatively low, ammonia can be added
Water management pH value 6.0-7.0, that is, configured optical fiber electroplating solution.
Further, the process conditions of the step 4 are：20 DEG C or so of temperature, pH value 7.0 or so, if pH value is relatively low,
Ammoniacal liquor regulation can be added, electroplates 20-30min.
Embodiment 1
A kind of fibre optical sensor metallization packaged method and technique, including Pre-treatment before plating, sensitization and activation, chemical nickel plating
With four parts such as plating metal, make optical fiber surface that there is certain catalytic activity in described Pre-treatment before plating, pretreatment into
Work(whether directly influence overlay coating quality and coating and optical fiber surface between adhesion, to prepare good coating, this
Invention establishes the pretreating process of complete set, including：Remove optical fiber sealer, cleaning, oil removing, cleaning, removal metal
Ion, cleaning, chemistry roughening, cleaning, heat treatment；, will be to be plated in described sensitization and activation using leaching catalytic metal activation method
Matrix infiltrates in the reducing agent and oxidizing agent solution prepared respectively, by redox reaction by the gold with catalytic activity
Category ion, which reduces from solion and is deposited in matrix surface, forms layer of metal catalytic film；Exist in described chemical nickel plating
One layer of fine and close, good Ni-P film of associativity is formed on optical fiber and FBG surfaces, is provided safeguard for follow-up plating metal；
The plating metal configuration electrogalvanizing, copper, gold solution, control in optimum process condition, obtain being coated with the grating of different metal.
The present invention is tested key parameters such as the temperature of the FBG after metallization and strains.Due to the thermal expansion of metal
Coefficient is larger, such as the thermal coefficient of expansion maximum 35 of metallic zinc-6℃-1, quartzy thermal coefficient of expansion is only 0.55-6℃-1, therefore gold
Category plated film serves the effect of temperature sensitizing, improves the temperature control of sensor；Simultaneously after plating metal, FBG strain
The relatively naked grating of coefficient has different degrees of raising.Therefore, the present invention realizes optical fiber FBG temperature sensitizing and strain sensitization,
It is a kind of metallization packaged that is effective, having certain application value that chemical plating, which is demonstrated, with reference to plating.
Meanwhile in actual applications, grating is pasted onto in metal structure by generally use adhesive, optical-fiber intelligent gold is formed
Belong to structure, appearance can not be completely fixed, and the defects of wriggling during force acting on transducer, make measurement data distortion.Using chemical plating
It the method for welding can be used to be fixed on object with reference to the FBG of plating metal packaging technology, there is associativity is good, air-tightness is good etc.
Advantage, and metal and metallic compound have the performance such as high temperature resistant, corrosion-resistant, extend FBG service life, expand its use
Scope.
The manufacturing process of the present invention is as follows：
Step 1 optical fiber Pre-treatment before plating：
(1-1) deprotects layer：The method being combined using chemical immersion and mechanical stripping.Prepare the 98wt% concentrated sulfuric acid,
Grating is immersed into solution 5-15min, dissolving FBG grid regions overlay；Matrix after taking-up processing is further light with optical fiber hoe scaler
Fiber coating layer is lightly removed, then picks alcohol with cotton balls or acetone gently wipes 4-6 times, finally in deionized water with ultrasound
Clean 5min；
(1-2) oil removing：In optical fiber and grating sensor preparation and end processing sequences, inevitably have greasy dirt and glue
It is attached to optical fiber surface.It is more commonly used in the lab and cheap in view of NaOH solution, optical fiber part to be plated is immersed in
20min in the NaOH solution that concentration is 20wt%；It is respectively placed in again in absolute ethyl alcohol and deionized water after taking-up and is cleaned by ultrasonic 5-
10min；
(1-3) removes metal ion：Remove the metal and metal ion that surface is stained with preparation and processing procedure.Prepare
HNO3：H2O=1:1 salpeter solution, pending optical fiber and FBG are put into 5-10min in the salpeter solution diluted, taken out
Optical fiber immersion is cleaned into 3min with ultrasonic wave in deionized water afterwards, the removal of impurities of metal and metal ion can be completed；
The roughening of (1-4) chemistry：Chemistry roughening essence is to carry out corrosion treatment to FBG surfaces, and it can become matrix surface
Micro-rough is obtained, makes surface that there is very strong adsorptivity.Coarsening time, temperature, the pH value of coarsening solution can influence to be roughened effect,
Wherein influence of the coarsening time to coating is maximum, and temperature and pH value are taken second place.Comprehensive every factor, the present invention use mixed acid, contained
There are hydrofluoric acid or F-Strongly acidic solution weak corrosion 3min is carried out to quartzy FBG；
(1-5) is heat-treated：The complete silicon-oxy tetrahedron structure in FBG surfaces is by a certain degree of destruction, surface after roughening
Silicon is in a kind of unstable state that can be obtained electronics or lose electronics.Therefore, when it is contacted with water, easily reaction
Silanol is generated, makes the thickness of moisture film continue to increase.And optical fiber is heat-treated after being roughened, this layer of moisture film can be removed, to increase
The adhesion and integrality of strong coating.Heat treatment purpose mainly go to remove water, treatment temperature is too high, FBG can by it is erasable fall, so
As long as treatment temperature is more than 100 DEG C.
Step 2 is sensitized and activation key step is as follows：
(2-1) is by 10g/L SnCl2Solution is added in 40ml/L hydrochloric acid, after stirring, sensitizing solution is formed, then in 30-
Under 40 DEG C of constant temperature, optical fiber is immersed in 15min in sensitizing solution, is finally cleaned by ultrasonic 2min in deionized water；
1g/L palladium chloride solution is added in 10ml/L hydrochloric acid by (2-2) is made activating solution, keeps sensitization constant temperature bar
Part, the optical fiber after sensitization is placed in copper chloride and hydrochloric acid configures in the activating solution formed and handles 20min.
Step 3 chemical nickel plating
(3-1) chemical nickel-plating liquid is mainly made up of main salt, reducing agent, complexing agent, buffer and stabilizer, the work of each component
With and its selection it is as follows：Main salt mainly provides nickel ion, and the most frequently used nickel salt has two kinds of nickel sulfate and nickel chloride, due to nickel sulfate
It is cheap, and be easily formed the higher product of purity, the present invention is from nickel sulfate as main salt；Reducing agent is mainly by main salt
Nickel ion be reduced into metallic nickel, it is deposited on FBG surface.In various common reducing agents, sodium hypophosphite price is low
Honest and clean, reduction effect is good, and toxicity and pollution are small, and this is using sodium hypophosphite as reducing agent；Complexing agent mainly enters with nickel ion
Row complexing reduces the concentration of free nickel ion, improves the stability of plating solution, herein using 85wt% lactic acid as complexing agent, simultaneously
It may also function as cushioning liquid pH effect；From boric acid as buffer, the pH value of plating solution is maintained, prevents from largely separating out during nickel plating
Hydrogen causes solution ph to decline；Stabilizer selects sodium fluoride, prevents plating solution selfdecomposition.
(3-2) configures chemical nickel-plating liquid, and the 85wt% lactic acid of measured amounts first, which is added in deionized water, to be mixed into
Enveloping agent solution, quantitative 30g/L nickel sulfates, 28g/L sodium hypophosphites, 35g/L boric acid and 30g/L chlorinations are then weighed respectively
Sodium is added in enveloping agent solution, finally adds ammoniacal liquor to adjust the pH value of plating solution.
(3-3) inserts 5-10min in chemical nickel-plating liquid under conditions of 20-25 DEG C, by optical fiber.
Step 4 electro-coppering：
The fiber grating that surface is had to the nickel-phosphorus alloy coating of conductive power is cleaned and dried with deionized water, is then fixed
On negative electrode.Anode uses graphite electrode, is first degreased with 10wt% NaOH solution.10wt%H is used again2SO4In solution
With then cleaned with distilled water, under given technique, be placed in electroplating solution and electroplate.
Copper electroplating solution is by 60g/L pyrophosphoric acids, 300g/L potassium pyrophosphate, the 40g/L hydrate of sodium potassium tartrate tetrahydrate four,
40g/L dipotassium hydrogen phosphates, 0.2g/L phytic acid, 0.1g/L vanillic aldehyde composition.In pH6.0-7.0,20 DEG C of temperature, electric current
0.5A/dm2Process conditions under, electroplate 20-30min, obtain the copper plating film of even compact.
Embodiment 2
Other handling process are same as Example 1, and difference is, gold-plating solution by 15-18g/L citric acids,
45g/L chlorauride, 35g/L potassium permanganate, 2g polishing agents composition.In pH6.5-7.0,25 DEG C of temperature, electric current 0.6A/dm2
Process conditions under, electroplate 30min, obtain the gold-plated film of even compact.
Embodiment 3
Other handling process are same as Example 1, and difference is, plating zinc solution is by 80g zinc sulfate, 6g boric acid,
2g polishing agents, 2g polishing agents form 200mL electroplating solution.Under 3V voltages, 25min is electroplated, obtains the zinc-plated of even compact
Film.
Embodiment 4
Specific metallization is analyzed as follows:
(1) influence of the pretreatment to coating：In theory, silica fibre surface coarsening can strengthen palladium ion and optical fiber matrix
Adhesion.Because silica fibre surface is after roughening, loss is produced, coarsening time is more long, and loss is bigger, and handles not
When being easy to phenomenon of rupture occur, this is unfavorable to practical application.Therefore, it is necessary to fixed chemical plating process parameter.
(2) influence of the soak time to coating：Nickel chemical plating technology condition is constant, and the fixed optical fiber roughening treatment time is
5min.Substantially coating is occurred without when being 5min between upon activation, the time increases to the continuity increase of coating after 10min, 20min
After can obtain uniformly continuous coating.Due to chemical Ni-plating layer, uniformly whether complete key is Metal Palladium particle in colloid palladium
Whether deposition is uniform, and soak time is longer, and it is more much more uniform that Metal Palladium particle is deposited on optical fiber surface, so as to which chemical Ni-plating layer is got over
It is uniformly complete.Therefore experiment determines soak time 20min.
(3) influence of the activation temperature to coating：Chemical Nickel Plating Parameters are constant, and the fixed optical fiber roughening treatment time is
5min, colloid palladium soak time are 20min.At 10 DEG C, coating can not be obtained substantially, and this is due to that temperature is too low, colloid palladium
Activity is relatively low, and with the rise of activation temperature, plating layer status gradually improves, and when activation temperature reaches 40 DEG C, can obtain good
Coating.But during more than 40 DEG C, obtain plating layer status and start to be deteriorated, this is due to temperature rise, and colloid palladium solution starts rotten mistake
The reason for effect.Therefore, optimal activation temperature should be controlled at 30-40 DEG C or so.
(4) influence of electroplating voltage, electroplating time to coating：Using a length of 55mm, a width of 15mm, thickness 0.02mm
Stainless steel substrates as flaky matrix, by setting different magnitudes of voltage, electroplating time, detection fiber and matrix combination situation.
9V, 5V and 3V are respectively set as shown in Figure 1, are changed electroplating time, are obtained the metal coating light under different situations
Grid comparison diagram.It can be seen that under 9V voltages, matrix surface generates seriously air flue phenomenon, and it is reliable can not to form dense uniform
Coating；Under 3V voltages, the plating time is fast on optical fiber matrix, and binding time is short, and bond strength is high, and coating more uniformly connects
It is continuous, it is considered as electroplating the ideal technology condition of optical fiber matrix.
As shown in Fig. 2 the SEM testing results of copper facing grating.Electroplate liquid is by 60g/L pyrophosphoric acids, 300g/L potassium pyrophosphate,
The 40g/L hydrate of sodium potassium tartrate tetrahydrate four, 40g/L dipotassium hydrogen phosphates, 0.2g/L phytic acid, 0.1g/L vanillic aldehyde composition.
In pH6.0-7.0,20 DEG C of temperature, electric current 0.5A/dm2Process conditions under, electroplate 20-30min, obtain the copper facing of even compact
Film.
As shown in figure 3, the SEM testing results of gold-plated grating.Electroplate liquid is by 15-18g/L citric acids, 45g/L chlorauride,
35g/L potassium permanganate, 2g polishing agents composition.In pH6.5-7.0,25 DEG C of temperature, electric current 0.6A/dm2Process conditions under, electricity
30min is plated, obtains the gold-plated film of even compact.
As shown in figure 4, the SEM testing results of zinc-plated grating.By 80g zinc sulfate, 6g boric acid, 2g polishing agents, 2g polishing agents
Form 200mL electroplating solution.Under 3V voltages, 25min is electroplated, obtains the zinc-plated film of even compact.
As shown in figure 5, metal coating grating temperature performance diagram.Gold-plated grating, zinc-plated grating, plating bronzing can be drawn
The temperature control coefficient of grid and naked grating is respectively 0.0117,0.0235,0.0169 and 0.0103, and gold, zinc, copper is hot swollen
Swollen coefficient difference 14.2-6℃-1、35-6℃-1、16.5-6℃-1, it can be seen that, because the thermal coefficient of expansion of metal is bigger, plate metal
Grating sensitivity it is higher.Its reason is due to temperature rise, surface metal stretching, necessarily should so as to be produced in grating grid region
Power, raster center wavelength produce drift under the collective effect of the stress and temperature, reach the effect of temperature sensitizing.Therefore, it is golden
Category plated film grating serves the effect of temperature sensitizing, improves the temperature control of sensor.
As shown in fig. 6, strain-gauge test platform schematic diagram.Cantilever beam is carbon fiber rectangular beam, and its size is length l=
150mm, width b=15mm, thickness h=0.7mm.
As shown in fig. 7, the emergent property curve map of metal coating grating.Four kinds of optical fiber FBG are fixed on cantilever beam upper table
Face, cantilever beam strain is adjusted by changing free end travel amount.Test result indicates that gold-plated optical fiber FBG, zinc-plated optical fiber FBG, plating
The bronzing fibre FBG coefficient of strain is 1.15 times, 1.09 times and 1.26 times of naked grid respectively, the FBG strains after this explanation plated film
Different degrees of raising be present in coefficient.The ductility of strain sensitivity and coated metal, coating structure, thickness of coating and coating
Metal is relevant with optical fiber bond strength.
The present invention is metallized using chemical plating with electroplating the method being combined to optical fiber, due to the thermal expansion system of metal
Number is larger, and metal coating serves the effect of temperature sensitizing, improves the temperature control of sensor；Simultaneously after plating metal,
The relatively naked grating of the FBG coefficient of strain has different degrees of raising.Therefore, the present invention realize optical fiber FBG temperature sensitizing and
Strain sensitization, it was demonstrated that chemical plating is a kind of metallization packaged technique that is effective, having certain application value with reference to plating.
Meanwhile in actual applications, there is the example of optical-fiber intelligent metal structure.The adhesive of generally use glues grating
It is attached in metal structure, appearance can not be completely fixed, and the defects of wriggling during force acting on transducer, make measurement data distortion.Adopt
The mode that welding can be used with the FBG of chemical plating combination galvanic metallization packaging technology is fixed on object, have associativity it is good,
The advantages that air-tightness is good, and metal and metallic compound have the performance such as high temperature resistant, corrosion-resistant, extend FBG service life,
Expand its use range.
The preferred embodiment of the application is the foregoing is only, is not limited to the application, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
- A kind of 1. fibre optical sensor metallization packaged method, it is characterised in that including：Optical fiber is pre-processed, is sensitized, is activated, chemical nickel plating, plating metal, is produced；The nickel liquid of the chemical nickel plating includes：Main salt nickel sulfate, reducing agent sodium hypophosphite, complexing agent 85wt% lactic acid, delay Electuary boric acid, stabilizer sodium fluoride；And ammoniacal liquor.
- 2. the method as described in claim 1, it is characterised in that the electroplating solution of the plating metal includes：Pyrophosphoric acid, burnt phosphorus Sour potassium, the hydrate of sodium potassium tartrate tetrahydrate four, dipotassium hydrogen phosphate, phytic acid, vanillic aldehyde, copper-bath, and ammoniacal liquor.
- 3. the method as described in claim 1, it is characterised in that the pretreating process includes：Deprotect layer, cleaning, oil removing, Cleaning, remove metal ion, cleaning, chemistry roughening, cleaning, heat treatment.
- 4. the method as described in claim 1, it is characterised in that SnCl is selected in described optical fiber surface sensitization and activation2With Cu points Metallic element not as sensitizer and with catalytic activity, using impregnation catalyst metal activation method, optical fiber surface is set to cover one Layer catalytic membrane.
- 5. the method as described in claim 1, it is characterised in that the plating metal, configure electroplate liquid in proportion, specific plating Regulation pH value to 7 or so, it is 20 DEG C in temperature during copper, electric current 0.5A/dm2Under conditions of, electroplate 20-30min.
- 6. method as claimed in claim 3, it is characterised in that the coarsening time is controlled in 3min or so, obtains surface light Slide, covering is good, complete uniform coating.
- 7. the method as described in claim 1, it is characterised in that activation temperature control is in 30-40 DEG C, soak time 20min。
- 8. the method as described in claim 1, it is characterised in that the chemical nickel plating concretely comprises the following steps：Measure first certain The 85wt% lactic acid of amount, which is added in deionized water, is mixed into enveloping agent solution, then weighs quantitative nickel sulfate, secondary Asia respectively Sodium phosphate, boric acid and sodium chloride are added in enveloping agent solution, finally add ammoniacal liquor to adjust the pH value of plating solution；At 20-25 DEG C Under conditions of, optical fiber is inserted into 5-10min in chemical nickel-plating liquid.
- 9. the method as described in claim 1, it is characterised in that the plating metal concretely comprises the following steps：Surface had into nickel The fiber grating of phosphor alloy coating is cleaned and dried with deionized water, is then attached on negative electrode；Anode uses graphite electrode, first Degreased with 10wt% NaOH solution；Mass concentration 10wt% H is used again2SO4Solution neutralizes, and is then cleaned with distilled water, Under given technique, it is placed in electroplating solution and electroplates 30min.
- 10. fibre optical sensor prepared by the method described in claim any one of 1-9.
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| CN113818013A (en) * | 2021-09-23 | 2021-12-21 | 镇江锦兴表面工程技术有限公司 | Surface treatment process for quartz optical fiber |
| CN113913821A (en) * | 2021-09-23 | 2022-01-11 | 镇江锦兴表面工程技术有限公司 | Surface treatment process for sapphire product |
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| CN113818013A (en) * | 2021-09-23 | 2021-12-21 | 镇江锦兴表面工程技术有限公司 | Surface treatment process for quartz optical fiber |
| CN113913821A (en) * | 2021-09-23 | 2022-01-11 | 镇江锦兴表面工程技术有限公司 | Surface treatment process for sapphire product |
| CN115992350A (en) * | 2021-10-19 | 2023-04-21 | 北京玻璃研究院有限公司 | Preparation method and device of compact and uniform gold-plated quartz optical fiber |
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