Background technology
Adopt the all-silica fiber pressure transducer of Fabry-Perot chamber interferometer principle to be formed by monox, heat shock resistance, corrosion-resistant, can under harsh environment, work.Wherein, the connected optical fiber external diameter of the physical dimension of microminiaturized all-silica fiber pressure transducer is identical.If use ordinary optic fibre communication silica fibre, external diameter only has 125 microns.Microminiaturized some special occasions that can be used for, as cardiovascular in this fibre optic compression sensor put in the diagnosis of cardiovascular obstruction, directly measure cardiovascular in ambulatory blood pressure everywhere, position and the order of severity stopped up in order to judgement.Also this pressure transducer and spark plug can be integrated, the dynamic pressure of measuring internal combustion engine changes to optimize the running parameter of engine, raises the efficiency, and reduces discharge.
Existing method for making is mainly operating as master with the welding based on fused quartz optical fiber and cleavage.Its basic manufacturing process is as follows: first, single mode silica fibre and one section of multimode silica fibre are welded together, near multimode optical fiber and single-mode fiber junction by multimode optical fiber cleavage.Due under certain condition, the corrosion rate of the covering of multimode optical fiber, much smaller than the corrosion rate of core, can retain clad section by the core corrosion of multimode optical fiber.Optical fiber after excessive erosion and other one section of optical fiber weld, and near weld by final stage optical fiber cleavage.Final stage optical fiber after cleavage will be served as pressure-sensitive film.The shapeliness size of the film that this method for making is made relies on fused fiber splice and cleavage to a great extent.Because the surperficial flatness of final stage optical fiber after welding inevitably can be affected, and surface after cleavage is also also imperfect.The position of cleavage can not accurately be controlled.Therefore, the thickness of the film of the making of this method is thicker, and repeatability is very poor, is not suitable for highly sensitive application and batch production.
For reducing film thickness and improving film quality, some are suggested based on improving one's methods of the method.First,, after cleavage, can further reduce the thickness of film with the film that the corrosion continuation corrosion that contains hydrofluorite is made.But because the initial conditions of film is not fine, although follow-up corrosion process can further reduce the thickness of film, minimum film thickness still can not meet highly sensitive application.Another is improved one's methods is before corrosion, first with traditional finishing method, the outside surface of film is thrown and is put down, and is then carrying out hydrofluorite corrosion, and adopts the thickness of the System Implementation monitoring film of a set of on-line monitoring.The thickness of the film that this method can be made may diminish to 2 microns.But, this method for making process complexity, poor repeatability, cost is high.
For improving the homogeneity of film and the thickness of reduction film, the method for the direct high temperature bonding of optical fiber after silicon oxide film and corrosion is suggested.Because film is to make after removing silicon after the silicon chip thermal oxide after polishing, the homogeneity of its material and the homogeneity of thickness are much better than method for making above.Therefore the method has good repeatability.The colorimetric sensor films of making is even, and film thickness can be less than 1 micron.Along with the attenuating of film thickness, because causing the probability of breakage of thin film applied, film and other object contacts also greatly increase.
In addition, in the manufacturing process of Fibre Optical Sensor, the plastic protective layer of optical fiber need to divest to realize the welding of optical fiber, cleavage and high temperature bonding.And it is very fragile without the optical fiber of plastic protective layer, easily broken.Therefore after completing, sensor production needs to apply protection.But because the making of plastic protective layer can not affect film, the pollution that do not have on film, therefore this safeguard measure is implemented more difficult.
In view of this, provide a kind of method for making of total oxygen SiClx optical fiber pressure/sound transducer to necessitate.
Summary of the invention
Goal of the invention of the present invention is to provide a kind of method for making of total oxygen SiClx optical fiber pressure/sound transducer; it is consistent with fibre diameter that the Fibre Optical Sensor that uses the method to make has size; film is even; reproducible; film protection mechanism and the armor coated operability that improves Fibre Optical Sensor, and do not affect the performance of sensor.
To achieve these goals, the method for making of a kind of Fibre Optical Sensor provided by the invention, it comprises the steps: S1: prepare material, comprise that silicon oxide film, one end have quartz glass optical fiber and the quartz glass capillary of cavity; S2: described silicon oxide film is placed on to described quartz glass capillary and described quartz glass optical fiber has between the end face of described cavity, to described silicon oxide film, described quartz glass capillary and described quartz glass optical fiber joint spot heating, above-mentioned silicon oxide film, quartz glass capillary and quartz glass optical fiber are bonded together; S3: remove unnecessary silicon oxide film; S4: by exposed quartz glass capillary and quartz glass optical fiber outside surface coating protective seam; Near S5: quartz glass capillary is cut off bonding place; S6: complete the making of Fibre Optical Sensor.
The method for making of the silicon oxide film of preparing in step S1 further, is as follows: S111: by silicon face deposit one deck silicon oxide film of twin polishing; S112: by the partial oxygen SiClx of photoetching and the above-mentioned silicon one side of erosion removal; S113: by corrosion, get rid of the silicon of not oxidated silicon protection; S114: the silicon oxide film that obtains silicon chip frame supported.
The method for making of the quartz glass capillary of preparing in step S1 further, is as follows: S121: quartz glass capillary is removed to polymer protective layer; S122: this quartz glass capillary of cleavage; S123: the quartz glass capillary that obtains flat end face.
The method for making of the quartz glass optical fiber of preparing in step S1 further, is as follows: S131: by common single mode quartz glass optical fiber and quartz glass capillary welding; S132: complete after welding, near cleavage quartz glass capillary weld, and remain a bit of quartz glass capillary; S133: the quartz glass optical fiber that must arrive one end and have cavity.
The method for making of the quartz glass optical fiber of preparing in step S1 further, can also be as follows: S141: by common single mode quartz glass optical fiber and the welding of multimode quartz glass optical fiber; S142: complete after welding, near cleavage multimode quartz glass optical fiber weld, and remain a bit of multimode quartz glass optical fiber; S143: one end of single mode quartz glass optical fiber is entered in hydrofluorite and corroded, dry up through deionized water rinsing and with nitrogen after taking-up; S144: the quartz glass optical fiber that must arrive one end and have cavity.
Further, the bonding step in step S2 is as follows: S201: quartz glass optical fiber and quartz glass capillary are put into respectively to two zirconium oxide ceramic contact pins, and the end face of quartz glass optical fiber and quartz glass capillary exposes outside ceramic contact pin; S202: two zirconium oxide ceramic contact pins are fixed on fixture, make quartz glass optical fiber parallel with quartz glass capillary end face and coaxial by alignment jig; S203: silicon oxide film is placed between quartz glass optical fiber and quartz glass capillary, and applies the power of about 0.05N-5N, make quartz glass optical fiber and quartz glass capillary clamp above-mentioned silicon oxide film; S204: above-mentioned quartz glass optical fiber, quartz glass capillary and silicon oxide film are heated to 700 DEG C-850 DEG C, continue after 1s-10s to stop exerting pressure, stop heating after stopping applying power 0-10 second.
Further, the bonding step in step S2 can also be as follows: S211: by quartz glass optical fiber and quartz glass capillary, put into respectively two V-shaped grooves, and expose respectively about 10-300 micron long quartz glass optical fiber and quartz glass capillary; S212: one of them V-shaped groove is fixed on the adjusting bracket of the adjustable power of an applying size, another V-shaped groove is fixed on an adjusting bracket, by regulating above-mentioned two adjusting brackets, make the end face of quartz glass optical fiber and quartz glass capillary parallel to each other and coaxial; S213: silicon oxide film is placed between quartz glass optical fiber and quartz glass capillary, and applies the power of about 0.05N-5N, make quartz glass optical fiber and quartz glass capillary clamp above-mentioned silicon oxide film; S214: above-mentioned quartz glass optical fiber, quartz glass capillary and silicon oxide film are heated to 700 DEG C-850 DEG C, continue after 1s-10s to stop exerting pressure, stop heating after stopping applying power 0-10 second.
Further, step S3 comprises the steps: S301: with the silicon oxide film outside method removal quartz glass optical fiber and the quartz glass capillary external diameter of machine cuts;
Further, step S3 also comprises the steps: S302: by the quartz glass optical fiber having welded, quartz glass capillary and silicon oxide film are put into hydrofluorite erosion liquid, erode unnecessary silicon oxide film.
Further, the method of the making silicon oxide film in step S111 comprises thermal oxidation method, low-pressure chemical vapor deposition method and plasma reinforced chemical vapor deposition method, while wherein using plasma reinforced chemical vapor deposition method, after thin-film deposition completes, use the method for high annealing, make silicon oxide film finer and close.
Further, the thickness of the making silicon oxide film in step S111 is 0.1um-10um.
Further, the silicon oxide film of the making in step S111 mixes in deposition process.
Further, the method for making of the protective seam in step S4 is as follows: S401: by the quartz glass optical fiber having welded, quartz glass capillary and silicon oxide film immerse in the mixed liquor of polymkeric substance and solvent; S402: good the welding that has applied polymkeric substance quartz glass optical fiber, quartz glass capillary and silicon oxide film are put into baking oven and toast.
Further, the method for cutting off quartz glass capillary in step S5 is cleavage method or meticulous emery wheel patterning method.
The method for making of a kind of Fibre Optical Sensor provided by the invention, has simplified the technology difficulty of the coating of polymer protective layer, and in coating procedure, without any need for the protection to film, it has improved the efficiency that Fibre Optical Sensor is made.Adopting quartz glass kapillary is as the Part III of device, and in the time of bonding, it has replaced ceramic substrate of the prior art; After bonding, before cleavage quartz glass capillary, carry out coating and the processing of polymer protective layer, after being disposed, carry out again cleavage quartz glass capillary, in polymkeric substance protective finish coating procedure, do not need silicon oxide film to carry out conservation treatment.In use frangibility not of the quartz glass optical fiber that obtains polymer protective layer protection, has improved security.And silicon oxide film front end remains with a bit of kapillary protection, and this silicon oxide film is unsuitable impaired, and the yield rate that it has improved Fibre Optical Sensor, has improved work efficiency.
Embodiment
Describe the present invention in detail below in conjunction with accompanying drawing, it illustrates principle of the present invention as the part of this instructions by embodiment, other aspects of the present invention, and feature and advantage thereof will become very clear by this detailed description.
The invention provides a kind of method for making of Fibre Optical Sensor, total oxygen SiClx optical fiber pressure/sound transducer of making by this method for making, can be for common pressure survey, can also be applied to some volumes to sensor and high-temperature stability and have the field of particular/special requirement (after one's own heart endovascular blood pressure measurement, in cylinder of internal-combustion engine the measurement of dynamic pressure etc.).As Figure 1-3, the method for making of a kind of Fibre Optical Sensor provided by the invention, it comprises the steps:
S1: prepare material, comprise that silicon oxide film 3, one end have quartz glass optical fiber 2 and the quartz glass capillary 1 of cavity 21;
S2: this silicon oxide film 3 is placed on to quartz glass capillary 1 and quartz glass optical fiber 2 has between the end face of cavity 21; To this silicon oxide film 3, quartz glass capillary 1 and quartz glass optical fiber 2 joint spot heating, this silicon oxide film 3, quartz glass capillary 1 and quartz glass optical fiber 2 are bonded together;
S3: remove unnecessary silicon oxide film 3;
S5: by armor coated to exposed quartz glass capillary 1 and quartz glass optical fiber 2 outside surfaces;
Near S6: quartz glass capillary 1 is cut off bonding place;
S7: complete the making of Fibre Optical Sensor.
The method for making of this Fibre Optical Sensor is made total oxygen SiClx optical fiber pressure/sound transducer specially, the external diameter of the quartz glass capillary 1 that it prepares in step S1 is identical with the external diameter of quartz glass optical fiber 2, this quartz glass optical fiber 2 was corroded, its one end has cavity 21, the diameter of this cavity 21 is connected with identical being convenient to of internal diameter of quartz glass capillary 1, the forming process of this cavity 21 will be discussed in more detail below, and quartz glass optical fiber 2 is single-mode fiber; The method for making of this silicon oxide film 3 will be described in detail below.
Silicon oxide film 3 is placed on to quartz glass capillary 1 to step S2 and quartz glass optical fiber 2 has between the end face of cavity 21, to prepare that it is carried out to bonding, (bonding is as by two surface cleaning, the homogeneity of atomically flating or heterogeneous semiconductor material are through surface clean and activation processing, directly combination under certain condition, pass through Van der Waals force, molecular force even atomic force becomes one bonding chip), the method for making of a kind of Fibre Optical Sensor provided by the invention is the improvement that the deficiency of the method based on existing fiber and silicon oxide film Direct Bonding is made, in the time of bonding, silicon oxide film is not to be placed on one through on the substrate surface of polishing, but be placed between the quartz glass optical fiber 2 and one section of quartz glass capillary 1 corroding.
In step S2, to silicon oxide film 3, quartz glass capillary 1 and quartz glass optical fiber 2 joint spot heating, this silicon oxide film 3, quartz glass capillary 1 and quartz glass optical fiber 2 are bonded together.By spot heating is carried out in silicon oxide film 3, quartz glass capillary 1 and quartz glass optical fiber 2 joints, temperature is greatly about 700 DEG C of-850 DEG C of left and right, can make above-mentioned silicon oxide film 3, quartz glass capillary 1 and quartz glass optical fiber 2 directly in conjunction with (by Van der Waals force, molecular force even atomic force bonding chip is become one) be integrated i.e. bonding.The mode of bonding has multiple, will specifically describe below.
Then remove unnecessary silicon oxide film 3 according to step S3, then carry out polymer-coated protective seam by step S4 and to exposed quartz glass capillary 1 and quartz glass optical fiber 2, to protect whole exposed quartz glass capillary 1 and quartz glass optical fiber 2.
Step S5 cuts off near quartz glass capillary 1 bonding place.Quartz glass capillary 1 after cut-out remains with a bit of kapillary, for silicon oxide film 3 is protected, makes it should not be impaired, and it has improved the yield rate of Fibre Optical Sensor.The method of cutting off quartz glass capillary in step S5 is cleavage method (cleavage is that mineral crystal breaks in a certain direction and produces smooth flat after stressed) or meticulous emery wheel patterning method.
Step S6, completes the making of whole total oxygen SiClx optical fiber pressure/sound transducer.
The method for making of a kind of Fibre Optical Sensor provided by the invention, adopting quartz glass kapillary 1 is as the Part III of device, and in the time of bonding, it has replaced ceramic substrate of the prior art; After bonding, before cleavage quartz glass capillary 1, carry out coating and the processing of polymer protective layer, after being disposed, carry out again cleavage quartz glass capillary 1, in polymkeric substance protective finish coating procedure, do not need silicon oxide film 3 to carry out conservation treatment.In use frangibility not of the quartz glass optical fiber 2 that obtains polymer protective layer protection, has improved security.And silicon oxide film 3 front ends remain with a bit of kapillary protection, this silicon oxide film 3 is unsuitable impaired, and the yield rate that it has improved Fibre Optical Sensor, has improved work efficiency.
As shown in Figure 4, the method for making of this silicon oxide film 3 is as follows:
S111: as shown in Fig. 4 a-4b, by the silicon of twin polishing 31 surface deposition one deck silicon oxide films 32;
Be specially, the silicon of 400 micron thick twin polishings 31 is placed on to 1100 degrees Celsius of lower wet-oxygen oxidations 6 hours, extremely the thickness of the oxide layer 32 (monox) on above-mentioned silicon chip two sides is roughly 0.1um-10um;
S112: as shown in Fig. 4 c, remove the partial oxygen SiClx 32 (exposing the breach 33 of a monox) of above-mentioned silicon 31 one sides by photoetching (photoetching technique) and corrosion (corrosion technology);
S113: as shown in Fig. 4 d, by corrosion (dry etching technology), get rid of the silicon 31 (exposing the breach 34 of a silicon chip 31) that not oxidated silicon 32 is protected;
S114: the silicon oxide film 3 that obtains silicon chip frame supported.
The method for making of this quartz glass capillary 1 is as follows:
S121: quartz glass capillary 1 is removed to polymer protective layer; S122: this quartz glass capillary 1 of cleavage; S123: obtain flat end face quartz glass capillary 1.
Wherein this quartz glass optical fiber 2 has two kinds of method for makings:
The first method for making, the method for making of this quartz glass optical fiber 2 can be:
S131: by common single mode quartz glass optical fiber 2 and quartz glass capillary 1 welding; S132: complete after welding, near cleavage quartz glass capillary 1 weld, and remain a bit of quartz glass capillary 1; S133: the quartz glass optical fiber 2 that must arrive one end and have cavity 21.
The second method for making, the method for making of quartz glass optical fiber can also be:
S141: by common single mode quartz glass optical fiber 2 and the welding of multimode quartz glass optical fiber; S142: complete after welding, near cleavage multimode quartz glass optical fiber weld, and remain a bit of multimode quartz glass optical fiber; S143: one end of single mode quartz glass optical fiber 2 is entered to corrosion in dense hydrofluorite (HF), rinse and dry up by nitrogen through ionized water after taking-up; S144: the quartz glass optical fiber 2 that must arrive one end and have cavity 21.
The a bit of quartz glass capillary 1 of above-mentioned residue is approximately 25 microns of left and right, remains a bit of multimode quartz glass optical fiber and is also approximately 25 microns of left and right; Above-mentioned one end by single mode quartz glass optical fiber 2 enters the corrosion time of about 3 minutes in dense hydrofluorite (HF).
Bonding step in step S2 also has two kinds of bonding methods:
The first bonding method: the bonding step in step S2 is as follows:
S201: quartz glass optical fiber 2 and quartz glass capillary 1 are put into respectively to two zirconium oxide ceramic contact pins 4, and the end face of quartz glass optical fiber 2 and quartz glass capillary 1 exposes outside ceramic contact pin 4;
The internal diameter of zirconium oxide ceramic contact pin 4 is 127 microns (as shown in Figure 5), and approximately 300 microns of the ends of exposing quartz glass optical fiber 2 and quartz glass capillary 1 are long;
S202: two zirconium oxide ceramic contact pins 4 are fixed on fixture. make quartz glass optical fiber 2 parallel and coaxial with quartz glass capillary 1 end face by alignment jig;
S203: silicon oxide film 3 is placed between quartz glass optical fiber 2 and quartz glass capillary 1, and applies the power of about 0.05N-5N, make quartz glass optical fiber 2 and quartz glass capillary 3 clamp above-mentioned silicon oxide film 3;
S204: above-mentioned quartz glass optical fiber 2, quartz glass capillary 1 and silicon oxide film 3 are heated to 700 DEG C-850 DEG C, continue after 1s-10s to stop exerting pressure, stop heating after stopping applying power 0-10 second.
The second bonding method: the bonding step in step S2 can also be as follows:
S211: by quartz glass optical fiber 2 and quartz glass capillary 1, put into respectively two V-shaped grooves, and expose respectively the long quartz glass optical fiber 2 of about 10-300 micron and quartz glass capillary 1;
S212: one of them V-shaped groove is fixed on the adjusting bracket of the adjustable power of an applying size, another V-shaped groove is fixed on an adjusting bracket, by regulating above-mentioned two adjusting brackets, make the end face of quartz glass optical fiber 2 and quartz glass capillary 1 parallel to each other and coaxial;
S213: silicon oxide film 3 is placed between quartz glass optical fiber 2 and quartz glass capillary 1, and applies the power of about 0.05N-5N, make quartz glass optical fiber 2 and quartz glass capillary 1 clamp above-mentioned silicon oxide film 3;
S214: above-mentioned quartz glass optical fiber 2, quartz glass capillary 1 and silicon oxide film 3 are heated to 700 DEG C-850 DEG C, continue after 1s-10s to stop exerting pressure, stop heating after stopping applying power 0-10 second.
Above-mentioned steps S3 comprises the steps:
S301: with the silicon oxide film 3 outside method removal quartz glass optical fiber 2 and quartz glass capillary 1 external diameter of machine cuts; Be specially, cut away unnecessary silicon oxide film 3 by ceramic contact pin 4.
Step S3 also comprises the steps:
S302: by the quartz glass optical fiber having welded 2, quartz glass capillary 1 and silicon oxide film 3 are put into hydrofluorite erosion liquid, erode unnecessary silicon oxide film 3.Be specially, by hydrofluorite (HF) erosion liquid, erode unnecessary silicon oxide film 3.
The method of the making silicon oxide film 3 in step S111 comprises thermal oxidation method, low-pressure chemical vapor deposition method and plasma reinforced chemical vapor deposition method, while wherein using plasma reinforced chemical vapor deposition method, after thin-film deposition completes, use the method for high annealing, make silicon oxide film finer and close.
The silicon oxide film 3 of the making in step S111 mixes in deposition process, to reach the object that changes property of thin film.The thickness of the silicon oxide film 3 of its manufacturing is 0.1um-10um.
The method for making of the protective seam in step S4 is as follows: S401: by the quartz glass optical fiber having welded 2, quartz glass capillary 1 and silicon oxide film 3 immerse in the mixed liquor of polymkeric substance and solvent; S402: the quartz glass optical fiber 2 good welding that has applied polymkeric substance, quartz glass capillary 1 and silicon oxide film 3 are put into baking oven and toast.Be specially, after exposed quartz glass capillary 1 and quartz glass optical fiber 2 are soaked in 5 seconds in photoresist, take out and put into baking oven Program and be warming up to 250 degrees Celsius of bakings 3 hours
People, in the time using the endovascular blood pressure of fiber sensor measuring, need to be positioned over sensor the position that needs measurement by wire, as cardiovascular, therefore, the volume of sensor is the smaller the better.The sensor being placed in cylinder of internal-combustion engine needs high temperature resistant, corrosion-resistant.
By the method for making of a kind of Fibre Optical Sensor provided by the invention, a kind of total oxygen SiClx optical fiber pressure/sound transducer of making, its identical with the external diameter of optical fiber (125 microns, do not comprise polymer-coated layer), therefore can more conveniently insert can be for common pressure survey.And the sensitive part of this sensor forms by quartz glass, and volume is little, has high temperature resistantly, corrosion-resistant, and the feature of fast response time, can also be applied to the dynamic pressure measurement in the cylinder of internal combustion engine etc. technical field.
The method for making of a kind of Fibre Optical Sensor provided by the invention, has simplified the technology difficulty of the coating of polymer protective layer, and in coating procedure, without any need for the protection to film, it has improved the efficiency that Fibre Optical Sensor is made.Adopting quartz glass kapillary is as the Part III of device, and in the time of bonding, it has replaced ceramic substrate of the prior art; After bonding, before cleavage quartz glass capillary, carry out coating and the processing of polymer protective layer, after being disposed, carry out again cleavage quartz glass capillary, in polymkeric substance protective finish coating procedure, do not need silicon oxide film to carry out conservation treatment.In use frangibility not of the quartz glass optical fiber that obtains polymer protective layer protection, has improved security.And silicon oxide film front end remains with a bit of quartz glass capillary protection, and this silicon oxide film is unsuitable impaired, and the yield rate that it has improved Fibre Optical Sensor, has improved work efficiency.
Disclosed above is only preferred embodiment of the present invention, certainly can not limit with this interest field of the present invention, and the equivalent variations of therefore doing according to the present patent application the scope of the claims, still belongs to the scope that the present invention is contained.