CN100375907C - Wet chemical metallizing process for quartz optical fiber grating surface - Google Patents
Wet chemical metallizing process for quartz optical fiber grating surface Download PDFInfo
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- CN100375907C CN100375907C CNB2005100200865A CN200510020086A CN100375907C CN 100375907 C CN100375907 C CN 100375907C CN B2005100200865 A CNB2005100200865 A CN B2005100200865A CN 200510020086 A CN200510020086 A CN 200510020086A CN 100375907 C CN100375907 C CN 100375907C
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Abstract
The present invention relates to a wet chemical metallizing process for a quartz fiber grating surface, which forms an inorganic coating layer with micropores and microcracks on a smooth quartz glass fiber grating surface. After the coating layer forming a 'lock effect' is processed by drying, and opening micropores and microcracks are formed on the coating layer so as to reach the goal of roughening, because moisture and other organic solvent are vaporized. After the fiber grating surface forms an inorganic multipore coating layer for roughening, palladium chloride is activated, and fiber gratings with the inorganic multipore coating layer on the surface is immerged in palladium chloride aqueous solution. The palladium chloride aqueous solution soaks in cavities and the microcracks of the inorganic coating layer, and the surface of the inorganic coating layer is provided with O<-> dangling bonds; because of the action of electrostatic attraction, Pd<2+> ion is absorbed on inner walls of the cavities and the microcracks at the inorganic coating layer. After processed by roughening and deacidized with hydrogen gas or sodium borohydride water solution, the fiber gratings can be chemically plated with nickel and gold, and a plating layer surface which is plated is even and bright; the plating layer has strong adhesive force and weldability, and the present invention is an effective method adapting to the metallization of the fiber grating surface.
Description
Technical field:
The invention belongs to the technology that quartz optical fiber grating surface is coated with ni-p alloy coating and metal level with wet chemical method.
Prior art:
The quartz glass optical fiber of mixing germanium and carrying hydrogen forms grating through Ultra-Violet Laser irradiation in fiber core, this grating is called as fiber grating.Fiber grating has become the important optical device of optical fiber communication and sensory field of optic fibre.Fiber grating need carry out gluing fixing when optical fiber communication and sensory field of optic fibre are used usually, or welds behind its surface metalation it is fixed.
Fiber grating is that the quartz glass optical fiber that adopts Ultra-Violet Laser irradiation to mix germanium and year hydrogen is made, and the essence of fiber grating surface metalation is exactly the quartz glass surface metalation.Because the quartz glass smooth surface forms the coat of metal and acquires a certain degree of difficulty; Fibre diameter is very little, and is easily broken after peelling off surperficial organic protection layer; Fiber grating generally is the middle part that is made in long one section optical fiber, therefore can not take the method for plating on general workpiece to operate; Be coated with on the fiber grating surface in the process if deal with improperly, will produce stress in the optical fiber, the optical parametric of grating will change and lose using value.
Existing technology is with the fine surface coarsening of quartz glass, and the method that adopts is with containing F usually
-Or H
2SiF
6Aqueous solution (volume ratio is generally HF: H
2SiF
6: H
2O=1: 1: 2) the quartz glass optical fiber surface is corroded, thereby make the quartz glass optical fiber surface coarsening, but this method of roughening has very big damage to the fiber grating surface, its tensile strength is reduced, and fracture easily, also be not easy to welding simultaneously, the conventional chemical plating will be passed through this step of stannous chloride sensitization usually in addition, owing to the easy oxidation in air of stannous chloride sensitizing solution was lost efficacy, thus can only use at short notice, thereby make troubles to continued operation.
Summary of the invention:
The present invention seeks to adopt the method that forms inorganic porous coating at quartz optical fiber grating surface to make its alligatoring, both formed the inorganic coating of band micropore and micro-crack on the surface of smooth quartz glass optical fiber grating, can form " snap close effect " and to also not causing damage in the fiber grating surface, owing to be to adopt wet chemical method to form coating on the quartz glass optical fiber surface, coating is after dried, because moisture content and other organic solvent evaporations, to form opening micropore and micro-crack on the coating, thereby reach the purpose of alligatoring.The fiber grating surface forms inorganic porous coating and after the alligatoring, activates with palladium bichloride again.Have the fiber grating of inorganic porous coating to immerse in the palladium chloride aqueous solution on the surface, palladium chloride aqueous solution will infiltrate in the hole and micro-crack of inorganic coating, and the inorganic coating surface has-0
-Unsettled strong, since the effect of electrostatic attraction, Pd
2+Ion will be adsorbed onto on the inwall of inorganic coating hole and micro-crack.After the palladium bichloride activation, reduce with hydrogen or sodium borohydride aqueous solution, adopt the method for hydrogen reducing to be, fast fiber grating is transferred in the container, prevent that palladium chloride aqueous solution on the fiber grating surface inorganic coating is at air drying, feed hydrogen rapidly, the maintenance regular hour can be with Pd behind the shutoff hydrogen
2+Reduction, quartz optical fiber grating is taken out in the reduction back, washes coating repeatedly with deionized water, removes the not firm Pd of surface adsorption, is that the method for available electroless plating is coated with ni-p alloy coating after the drying.Adopt sodium borohydride aqueous solution reduction Pd
2+Method be, after from palladium chloride aqueous solution, taking out quartz optical fiber grating, wash inorganic coating slightly with sodium borohydride aqueous solution, it is dry to put into drying box, prepares sodium borohydride aqueous solution then, and the fiber grating that drying is crossed is put into sodium borohydride aqueous solution and soaked, soak the back and take out quartz optical fiber grating, wash coating repeatedly with deionized water, remove the not firm Pd of surface adsorption, dry back is coated with ni-p alloy coating in its surface chemistry.
The present invention compares with the technology of using always now, has following characteristics:
1, with colloidal sol alligatoring is carried out on the fiber grating surface, can be avoided severe corrosive solution that the fiber grating surface is caused damage and reduced its tensile strength, can strengthen the adhesion of palladium particle simultaneously, thereby strengthen the adhesion of the coat of metal;
2, unsettled being good for by electrostatic attraction of inorganic coating surface-0-attracts Pd2+, and Pd2+ penetrates in inorganic coating hole and the micro-crack, can firm attachment also play catalytic action on inorganic coating after the reduction; " the snap close effect " of inorganic coating hole and micro-crack is obvious, and the adhesion on metal level that is coated with and fiber grating surface obviously is better than the adhesion of conventional method.
Description of drawings
Fig. 1, wet chemical metallizing process for quartz optical fiber grating surface process flow diagram
Embodiment
At first adopt wet chemical method to form inorganic porous coating on the quartz glass optical fiber surface, because the quartz glass optical fiber surface can be closed with titania, silicon dioxide valence bond, form Si-O-Ti, Si-O-Si key, so titania, the porous silica coating can be in quartz glass optical fiber surface firm attachment.At first need to prepare titania and silicon dioxide gel, TiO 2 sol can adopt prepared by tetrabutyl titanate hydrolysis, the step that adopts butyl titanate to prepare TiO 2 sol is that the 10-20mL butyl titanate is added in the 3-5mL isopropyl alcohol, the nitric acid of 2mL 70% is added in the deionized water of 150mL, mixed liquor with butyl titanate and isopropyl alcohol slowly is added drop-wise in the aqueous solution of nitric acid again, 75-80 ℃ of strong agitation, form TiO 2 sol.Silicon dioxide gel can be by the method preparation of hydrolysis ethyl orthosilicate (TEOS).Its basic step is, is solvent with ethanol (EtOH), HCl and NH
3H
2O is a catalyzer, earlier with H
2O and TEOS mix, stir by 2: 1 (volume ratio), use HCl catalysis simultaneously, regulate pH=2.0, add NH behind the 2h
3H
2O and H
2O/EtOH solution (volume ratio EtOH: H
2O=1: 1), regulate pH〉7.5, stir 2h and obtain silicon dioxide gel.
The quartz optical fiber grating cotton ball soaked in alcohol wiped clean that will need to do surperficial roughening treatment after titania, the silicon dioxide preparation, use 70% nitric acid dousing 5min again, water is rinsed well, 5-10min in the colloidal sol of immersion titania or silicon dioxide, take out and put into 120 ℃ of dry 10-30min of drying box, immersion plating and dry run repeat 2-6 time.Ground floor must be a titania during preparation, next is silicon dioxide layer, and the two replaces then, and outermost layer is a silicon dioxide layer.
The fiber grating surface forms inorganic porous coating and after the alligatoring, activates with palladium bichloride again.There is the fiber grating of inorganic porous coating to be immersed in the palladium chloride aqueous solution of the 0.1-0.3g/L for preparing on the surface, have the fiber grating of inorganic porous coating to immerse 5-10min in the palladium chloride aqueous solution on the surface, palladium chloride aqueous solution will infiltrate in the hole and micro-crack of inorganic coating.There is-0 unsettled being good on the inorganic coating surface, since the effect of electrostatic attraction, Pd
2+Ion will be adsorbed onto on the inwall of inorganic coating hole and micro-crack.Pd
2+Available hydrogen or sodium borohydride aqueous solution reduction, adopting the method for hydrogen reducing is fast fiber grating to be transferred in the container, prevent that palladium chloride aqueous solution on the fiber grating surface inorganic coating is at air drying, feed hydrogen rapidly, keep 20-60min behind the shutoff hydrogen, Pd
2+Reduction.Taking out fiber grating, wash coating repeatedly with ionized water, remove the not firm Pd of surface adsorption, is that the method for available electroless plating is coated with ni-p alloy coating after the drying.Adopt sodium borohydride aqueous solution reduction Pd
2+Method be, from palladium chloride aqueous solution, take out fiber grating after, wash inorganic coating slightly with deionization, put into 120 ℃ the dry 10-20min of drying box.Compound concentration is the sodium borohydride aqueous solution of 0.1-2.0g/L, the fiber grating that drying is crossed is put into sodium borohydride aqueous solution 2-5min, take out fiber grating, wash coating repeatedly with deionized water, remove the not firm Pd of surface adsorption, dry back is coated with ni-p alloy coating in its surface chemistry.Can carry out chemical nickel plating and chemical gilding through alligatoring with the fiber grating after hydrogen or the sodium borohydride aqueous solution reduction processing.The method of electroless plating is with 20～35g/L nickelous sulfate; 15～25g/L inferior sodium phosphate; Respectively with deionized water dissolving and mixing (remembering that this mixed liquor is A); Get 3～5ml/L lactic acid and add water and add 2～6g/L sodium carbonate again and stir, stir the back and add 3～5g/L ammonium chloride and 1～2mg/L asccharin.Stir and obtain mixed liquid B.B liquid is added in the A solution, add 84 ℃ of deionized water temperature while stirring; Transfer pH=4.4-4.8 at last.
Embodiment
Electroless plating embodiment 1
30g nickelous sulfate and 20g inferior sodium phosphate are also mixed (remembering that this mixed liquor is A) with the 100mL deionized water dissolving respectively; Measure 4mL lactic acid and add water to 200mL, add 3g sodium carbonate, stir 10min, add 4g ammonium chloride and 1mg asccharin, stirring obtains mixed liquid B.B liquid is added in the A solution, add deionized water while stirring, transfer pH=4.4-4.8 at last to 1000mL.
Chemical nickel plating embodiment 2:
But plating bath compound method reference example 1, it is as follows that lactic acid is changed to the concrete parameter of sodium citrate, sodium acetate:
Nickelous sulfate 30g/L;
Inferior sodium phosphate 20g/L;
Sodium citrate 20g/L;
Sodium acetate 10g/L;
Asccharin 1mg/L;
84 ℃ of temperature;
PH value 4.4-4.8
Behind fiber grating plating nickel on surface phosphorus alloy, in order to improve its weldability, need be on the nickel-phosphorus alloy coating surface chemical gilding, its parameter is as follows:
Potassium auricyanide 5g/L;
Ammonium chloride 24g/L;
Sodium citrate 16g/L;
Inferior sodium phosphate 3g/L;
Sodium carbonate 6g/L;
84 ℃ of temperature;
PH value 7.0-7.5
Technology of the present invention is simple, easy to operate, and the lip-deep coat of metal of fiber grating has very strong adhesion and good weldability, and the metallization packaged and the practicability that can be fiber grating are laid a good foundation.
Claims (5)
1. wet chemical metallizing process for quartz optical fiber grating surface is characterized in that:
Step 1: before carrying out chemically plating, form the inorganic non-metallic porous coating at quartz optical fiber grating surface and make this surface coarsening, wherein, this inorganic non-metallic porous coating is the porous coating that titanium dioxide layer and silicon dioxide layer alternately form;
Step 2: after the alligatoring surface is had the fiber grating of this coating to immerse in the palladium chloride aqueous solution and activate, palladium chloride aqueous solution will infiltrate in the hole and micro-crack of this coating, owing to the effect of electrostatic attraction, Pd
2+Ion will be adsorbed onto on the inwall of this coating hole and micro-crack;
Step 3: after the palladium bichloride activation, reduce with hydrogen or sodium borohydride aqueous solution;
Step 4: quartz optical fiber grating is taken out in the reduction back, washes coating repeatedly with deionized water, removes the not firm Pd of surface adsorption, is that the method for available electroless plating is coated with ni-p alloy coating and gold layer after the drying.
2. a kind of wet chemical metallizing process for quartz optical fiber grating surface according to claim 1, described step 1 is characterised in that: at first need to prepare TiO 2 sol and silicon dioxide gel, the quartz optical fiber grating cotton ball soaked in alcohol wiped clean that will need to do surperficial roughening treatment after TiO 2 sol and the silicon dioxide gel preparation, use 70% nitric acid dousing 5min again, water is rinsed well, 5-10min in the colloidal sol of immersion titania or silicon dioxide, take out and put into 120 ℃ of dry 10-30min of drying box, immersion plating and dry run repeat 2-6 time; Ground floor must be a titanium dioxide layer during preparation, next is silicon dioxide layer, and the two replaces then, and outermost layer is a silicon dioxide layer.
3. a kind of wet chemical metallizing process for quartz optical fiber grating surface according to claim 2, it is characterized in that: the method for preparing TiO 2 sol is: 10～20mL butyl titanate is added in 3～5mL isopropyl alcohol, the nitric acid of 2mL 70% is added in the deionized water of 150mL, mixed liquor with butyl titanate and isopropyl alcohol slowly is added drop-wise in the aqueous solution of nitric acid again, 75～80 ℃ of strong agitation, form TiO 2 sol; The method for preparing silicon dioxide gel is: be raw material with the ethyl orthosilicate, ethanol is solvent, HCl and NH
3H
2O is a catalyzer, earlier with H
2O and TEOS mix, stir by 2: 1 volume ratios, use HCl catalysis simultaneously, regulate pH=2.0, add NH behind the 2h
3H
2O and H
2O/EtOH solution, volume ratio EtOH: H
2O=1: 1, regulate pH＞7.5, stir 2h and obtain silicon dioxide gel.
4. a kind of wet chemical metallizing process for quartz optical fiber grating surface according to claim 1, it is characterized in that: the consisting of of employed chemical nickel-plating liquid in the method for described electroless plating: nickelous sulfate 30g/L, inferior sodium phosphate 20g/L, lactic acid 4ml/L, sodium carbonate 3g/L, ammonium chloride 4g/L, asccharin 1mg/L; Perhaps, nickelous sulfate 30g/L, inferior sodium phosphate 20g/L, sodium citrate 20g/L, sodium acetate 10g/L, asccharin 1mg/L.
5. a kind of wet chemical metallizing process for quartz optical fiber grating surface according to claim 1 is characterized in that consisting of of employed chemical gold plating liquid in the method for described electroless plating: potassium auricyanide 5g/L; Ammonium chloride 24g/L; Sodium citrate 16g/L; Inferior sodium phosphate 3g/L; Sodium carbonate 6g/L.
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| CN100375907C true CN100375907C (en) | 2008-03-19 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103334095B (en) * | 2012-10-15 | 2016-07-20 | 上海应用技术学院 | A kind of chemical nickel-plating liquid and application thereof |
| CN103628104B (en) * | 2013-11-28 | 2016-04-06 | 中国建筑材料科学研究总院 | The optical fiber of optical fiber surface method for metallising, surface metalation and application thereof |
| CN104406625A (en) * | 2014-10-29 | 2015-03-11 | 安徽省科普产品工程研究中心有限责任公司 | Preparation method of nickel-plated fiber grating sensor |
| US11673831B2 (en) * | 2019-10-01 | 2023-06-13 | The Hong Kong University Of Science And Technology | Method for preparing optical fibers with high-particle-coated porous polymeric outer coating layers |
| CN111427115B (en) * | 2020-04-13 | 2021-09-10 | 武汉理工大学 | Surface modified metal coating optical fiber and preparation method and preparation system thereof |
| CN113307511B (en) * | 2021-06-11 | 2022-06-28 | 中国建筑材料科学研究总院有限公司 | Quartz optical fiber and preparation method and device thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0539581A (en) * | 1991-08-05 | 1993-02-19 | Ishikawajima Harima Heavy Ind Co Ltd | Production of electromagnetic shield material |
| JPH05257067A (en) * | 1992-03-13 | 1993-10-08 | Fujikura Ltd | Metal coated image fiber |
| JP2004084013A (en) * | 2002-08-27 | 2004-03-18 | Japan Science & Technology Corp | Electroless plating method and optical probe |
-
2005
- 2005-12-20 CN CNB2005100200865A patent/CN100375907C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0539581A (en) * | 1991-08-05 | 1993-02-19 | Ishikawajima Harima Heavy Ind Co Ltd | Production of electromagnetic shield material |
| JPH05257067A (en) * | 1992-03-13 | 1993-10-08 | Fujikura Ltd | Metal coated image fiber |
| JP2004084013A (en) * | 2002-08-27 | 2004-03-18 | Japan Science & Technology Corp | Electroless plating method and optical probe |
Non-Patent Citations (3)
| Title |
|---|
| 石英光纤表面化学镀镍磷合金工艺. 李小甫，姜德生，余海湖，余丁山，杨恩宇，李鸿辉.化工学报，第56卷第1期. 2005 * |
| 石英玻璃光纤表面化学镀镍. 李小甫，余海湖，姜德生，许丕池.光学与光电技术，第1卷第2期. 2003 * |
| 采用静电自组装技术在光纤上制备光学薄膜的研究. 余海湖，李小甫，许丕池，姜德生.光通信研究，第3期. 2002 * |
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Owner name: WUHAN PHYSICS AND ENGINEERING CONQUER CO., LTD. Free format text: FORMER OWNER: WUHAN UNIV. OF SCIENCE AND ENGINEERING Effective date: 20091218 |
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Effective date of registration: 20091218 Address after: Hubei city of Wuhan province Wuchang Luoshi Road No. 122 Patentee after: Wuhan Ligong Guangke Co., Ltd. Address before: Hubei city of Wuhan province Wuchang Luoshi Road No. 122 Patentee before: Wuhan University of Technology |