CN104195527B - Glass capillary plated surface carbon film device - Google Patents

Glass capillary plated surface carbon film device Download PDF

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Publication number
CN104195527B
CN104195527B CN201410470320.3A CN201410470320A CN104195527B CN 104195527 B CN104195527 B CN 104195527B CN 201410470320 A CN201410470320 A CN 201410470320A CN 104195527 B CN104195527 B CN 104195527B
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housing
carbon film
glass
collimation
glass capillary
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CN104195527A (en
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王昌
刘素香
王英英
刘小会
赵庆超
马龙
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Laser Institute of Shandong Academy of Science
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Laser Institute of Shandong Academy of Science
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Priority to CN201410470320.3A priority patent/CN104195527B/en
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Abstract

A kind of glass capillary plated surface carbon film device and technique, it comprises the CO 2 laser marking machine be fixed on base and the prism coordinated with CO 2 laser marking machine, also comprise the housing of a hollow, housing side is provided with the optical transmission window corresponding with prism, the first pore and the second pore is provided with in housing another side, first pore is communicated with vacuum pump, and the second pore is communicated with acetylene nitrogen gas tank; Housing is provided with fiber clamp, enclosure interior and hull outside hermetic seal.This plating carbon film device is applicable to chemical gaseous phase depositing process and carries out carbon film deposition at capillary glass tube-surface.Need the glass capillary of plated film to insert in collimation Glass tubing, its afterbody tail optical fiber tightens sealing by rubber pad, fiber clamp, optical fiber stationary fixture and nut, and two turriform piecing devices connect vacuum pump and gas tank respectively.The glass capillary of coating carbon film effectively can stop hydrionic corrosion in external environment, improves its work-ing life.

Description

Glass capillary plated surface carbon film device
Technical field
The invention belongs to fiber optic sensor technology field, relate to film coating apparatus and the technique of a kind of anti-hydrogen loss method of Fibre Optical Sensor, particularly a kind of capillary glass tube-surface.
Background technology
Need to carry out Real-Time Monitoring to downhole temperature, pressure and other parameters in oilfield development process, understand the physical condition of down-hole thus optimize oil recovery scheme, improve oil-production efficiency, due to the severe environment of down-hole, traditional electronic sensor cannot in the work of down-hole long-term stability, and the advantages such as Fibre Optical Sensor is strong, corrosion-resistant with its immunity from interference, unfailing performance is good are subject to applying more and more widely.
Nineteen eighty-three, N. Uchida describes the significant optical fiber attenuation change that is laid the optical cable more than 2 years in the literature, the focus that be worn to as people research of the optical fiber made in transmitting procedure, afterwards, by experiment and theoretical investigation learn, this be due to hydrogen molecule infiltrate fiber cores district, have an effect with the glass basis of optical fiber or form OH key, cause the phenomenon of added losses, " hydrogen loss " of the optical fiber be namely commonly called as.
Optical fiber downhole pressure-temperature sensor adopts F-P cavity pressure measurement, Fiber Bragg Grating FBG thermometric, F-P cavity adopts the quartz capillary with optical fiber same material, due in hydrionic environment, hydrogen ion can be diffused in quartz capillary, react with the defect in quartz capillary simultaneously, and then be diffused in optical fiber and cause the decay of optical signal transmission to increase, affect the measuring accuracy of Fibre Optical Sensor and the work-ing life of Fibre Optical Sensor, the permanent stability application of NdFeB permanent magnets to Fibre Optical Sensor therefore improving Fibre Optical Sensor has vital effect.
Physical method and chemical process two kinds is mainly contained in the method for optical fiber or quartz capillary surface coating, wherein physical method mainly contains thermal evaporation, sputtering method and ion plating method etc., chemical process is chemical Vapor deposition process mainly, the main method preventing optical fiber hydrogen loss by chemical Vapor deposition process at optical fiber or quartz capillary plated surface carbon film, chemical Vapor deposition process is exactly that two or more gaseous starting materials imports in a reaction chamber in theory, then there is chemical reaction each other in them, form a kind of new deposition of material to matrix surface.
Summary of the invention
The object of this patent is to provide a kind of device at quartz wool thin glass tube plated surface carbon film and technique, is placed in by quartz wool thin glass tube in a closed shell, passes through CO 2laser apparatus carries out local heating to quartz wool thin glass tube, its Heating temperature is by arranging laser energy and intensity regulates, adopt acetylene gas as reactant gases, first closed shell is vacuumized, the mixed gas of acetylene and nitrogen is passed into again in closed shell, at high temperature first acetylene gas carries out scission of link and dehydrogenation reaction, namely
Finally carbon film is formed by polyreaction repeatedly.
Technical scheme of the present invention is, a kind of glass capillary plated surface carbon film device, it comprises the CO 2 laser marking machine be fixed on base and the prism coordinated with CO 2 laser marking machine, also comprise the housing of a hollow, housing side is provided with the optical transmission window corresponding with prism, be provided with the first pore and the second pore in housing another side, the first pore is communicated with vacuum pump, and the second pore is communicated with acetylene nitrogen gas tank; Housing is provided with fiber clamp, enclosure interior and hull outside hermetic seal.
By arranging CO 2the mark length of laser marking machine and laser intensity and time, it can be regulated the Heating temperature of quartz wool thin glass tube; The effect of prism is horizontal direction by vertical laser refraction, enters housing by zinc selenide diaphragm.
The concrete feature of this programme also has, and described optical transmission window adopts zinc selenide diaphragm, and the effect of zinc selenide diaphragm has been to CO 2the anti-reflection effect of laser.
Vacuum pump is connected with housing by turriform joint, and its effect is vacuumized by housing; Acetylene nitrogen gas tank is also connected with housing by a turriform joint, is passed into the reactant gases of acetylene and nitrogen by turriform joint in housing.
Housing is provided with view port, and the eyeglass on view port is fixed on housing by high-temp glue, through the carbon film coating situation in window lens Real Time Observation housing;
Case top is provided with vent valve and tensimeter; Vent valve, is fixed by screw thread and sealing-ring and is sealed on housing, in order to relief pressure, and pressure in balance housing; Tensimeter is fixed by screw thread and silica gel and is sealed on housing, and in order to the pressure in Real-Time Monitoring housing, vent valve, in order to relief pressure, prevents dangerous generation.
Housing is fixed on the mobile platform of position by nut, and is connected with base by position mobile platform, and position mobile platform can carry out upper and lower, that front, rear, left and right are sextuple mobile fine setting relative to base, makes quartz wool thin glass tube be placed in CO in order to regulate 2the focus place of laser.
Fiber clamp comprises collimation Glass tubing permanent seat, collimation Glass tubing permanent seat comprises head, neck and afterbody, recess diameter is greater than head and afterbody, the head and afterbody side that collimate Glass tubing permanent seat are provided with sealing-ring, collimation Glass tubing permanent seat afterbody is inserted in case top stepped hole adaptive with it, collimation Glass tubing permanent seat afterbody lower end high-temp glue is stained with collimation Glass tubing, collimation Glass tubing internal diameter is suitable with the quartz wool thin glass tube external diameter that need plate carbon film, collimation Glass tubing is used for fixing quartz wool thin glass tube, collimation Glass tubing permanent seat head is set with intermediate sleeve, rubber cradle is provided with between intermediate sleeve and collimation Glass tubing permanent seat head, fastening nut is sleeved on and compresses intermediate sleeve with the thread fit on housing outside intermediate sleeve and realize hermetic seal.
Positioning convex intermediate sleeve is provided with on vertical chute and collimation Glass tubing permanent seat coordinates, and convex role makes intermediate sleeve and collimation Glass tubing permanent seat keep circumference location.
A technique for quartz wool thin glass tube surface-coated carbon film, it comprises the steps:
(1) previously described glass capillary plated surface carbon film device is used, by the collimation Glass tubing needing the glass capillary plating carbon film to be placed in fiber clamp bottom, tail optical fiber is through rubber cradle, tighten fastening nut, compress intermediate sleeve and rubber cradle, marked by the relative position of intermediate sleeve and housing, vacuum pump is connected with housing by turriform joint with acetylene nitrogen gas tank.
(2) go out distance between luminous point and prism and the prism of regulation of carbon dioxide laser marking machine are 22cm to the focal length that the distance sum of quartz wool thin glass tube is CO 2 laser marking machine, then carried out the fine setting of distance by position mobile platform, stop regulating when fine setting is maximum to the brightness being observed quartz wool thin glass tube by view port.
(3) open vacuum pump to bleed, be pumped to when tensimeter is shown as zero and close vacuum pump switch, open acetylene nitrogen gas tank switch, pass into reactant gases, ventilate after about 3 minutes, open vacuum pump switch limit and pass into reactant gases limit and bleed, to guarantee to be full of reactant gases in housing, there is no air, then vacuum pump cuts out.
(4) opening CO 2 laser marking machine setting mark figure is rectangle, length is about 5cm, when regulation of carbon dioxide laser marking machine mark intensity is about 300bit, start to carry out mark, namely carbon dioxide laser is to the heating of quartz capillary, because marking image is rectangle, laser can carry out mark to the total length of quartz wool thin glass tube, avoids the heating that when also needing glass capillary is moved up and down when adopting the heating of laser apparatus single-point laser, disalignment causes uneven; While mark heating, reactant gases decomposes, and carbon film is deposited on the surface of glass capillary, to glass capillary mark 2 ~ 3 times, stops mark.
(5) positioning convex intermediate sleeve is provided with on vertical chute and collimation Glass tubing permanent seat coordinates, and convex role makes intermediate sleeve and collimation Glass tubing permanent seat keep circumference location.
(6) be labeled as basis with the relative position of intermediate sleeve and housing, with spanner, intermediate sleeve is rotated clockwise 180 °, carry out local heating plating carbon film to the other one side of glass capillary, method is the same.
(7) after glass capillary both sides carbon film has deposited, first vacuum pump is opened and the acetylene reaction gas in housing is extracted out, then turn on fastening nut, fiber clamp is taken out, taken out from collimation Glass tubing by the glass capillary of plating carbon film, so far glass capillary plated surface carbon film completes.
The beneficial effect of this programme is: this device adopts CO 2 laser marking machine as LASER Light Source, utilize CO 2 laser marking machine can mark one segment length, the heating that when avoiding also needing quartz wool thin glass tube is moved up and down when adopting the heating of laser apparatus single-point laser, disalignment causes be uneven.This device compresses collimation Glass tubing permanent seat by screwing fastening nut, and due to through hole rubber cradle having diameter be slightly less than fibre diameter, extruding rubber cradle realizes the sealing to optical fiber.Two turriform piecing devices realize vacuumizing and the sealing of ventilate body timer and flexible pipe, by the pressure in tensimeter Real-Time Monitoring housing, utilize vent valve releasing device internal pressure.Zinc selenide eyeglass plays enhancement to carbon dioxide laser, reduces the power loss of carbon dioxide laser, realizes the local heating of carbon dioxide laser to glass capillary.
Accompanying drawing explanation
Fig. 1 is glass capillary plated surface carbon film device schematic diagram.Fig. 2 is glass capillary plated surface carbon film device local section structural representation.Fig. 3 is quartz wool thin glass tube and afterbody optical fiber sealing device enlarged diagram.
In figure, 1-CO 2 laser marking machine; 2-prism; 3-vacuum pump; 4-acetylene nitrogen gas tank; 5-zinc selenide diaphragm; 6-view port; 7-position mobile platform; 8-housing; 10-vent valve; 11-tensimeter; 12-fastening nut; 13-intermediate sleeve; 14-fiber clamp; 15-collimates Glass tubing; 16-rubber cradle; 17-positioning convex; 18-glass capillary; 19-tail optical fiber; 20-collimates Glass tubing permanent seat; 21-first pore; 22-second pore; 23-sealing-ring; 24-stepped hole.
Embodiment
In conjunction with the technical program and drawings in detail, apparatus of the present invention and the method implementation process at quartz wool thin glass tube surface-coated carbon film is described.
Embodiment 1:
As shown in Figure 1-2, a kind of glass capillary plated surface carbon film device, it comprises the CO 2 laser marking machine 1 be fixed on base and the prism 2 coordinated with CO 2 laser marking machine 1, also comprise the housing 8 of a hollow, housing 8 one sides are provided with the optical transmission window corresponding with prism 2, be provided with the first pore 21 in housing 8 another side and the second pore 22, first pore 21 is communicated with vacuum pump 3, the second pore 22 is communicated with acetylene nitrogen gas tank 4; Housing 8 is provided with fiber clamp 14, housing 8 inside and the outside hermetic seal of housing 8.
By arranging the mark length of CO 2 laser marking machine 1 and laser intensity and time, it can be regulated the Heating temperature of glass capillary 18; The effect of prism 2 is horizontal direction by vertical laser refraction, enters housing 8 by zinc selenide diaphragm 5; Described optical transmission window adopts zinc selenide diaphragm 5, and the effect of zinc selenide diaphragm 5 has been to CO 2the anti-reflection effect of laser.
Vacuum pump 3 is connected with housing 8 by turriform joint, and its effect is vacuumized by housing 8; Acetylene nitrogen gas tank 4 is also connected with housing 8 by a turriform joint, is passed into the reactant gases of acetylene and nitrogen by turriform joint in housing 8.
Housing 8 is provided with view port 6, and the eyeglass on view port 6 is fixed on housing 8 by high-temp glue, through the carbon film coating situation in window lens 6 Real Time Observation housing 8;
Housing 8 top is provided with vent valve 10 and tensimeter 11; Vent valve 10 is fixed by screw thread and sealing-ring and is sealed on housing 8, in order to relief pressure, and pressure in balance housing 8; Tensimeter 11 is fixed by screw thread and silica gel and is sealed on housing 8, in order to the pressure in Real-Time Monitoring housing 8, prevents dangerous generation.
Housing 8 is fixed on position mobile platform 7 by nut, and be connected with base by position mobile platform 7, position mobile platform 7 can carry out upper and lower, that front, rear, left and right are sextuple mobile fine setting relative to base, makes glass capillary 18 be placed in CO in order to regulate 2the focus place of laser.
Fiber clamp 14 comprises collimation Glass tubing permanent seat 20, collimation Glass tubing permanent seat 20 comprises head, neck and afterbody, recess diameter is greater than head and afterbody, the head and afterbody side that collimate Glass tubing permanent seat 20 are provided with sealing-ring 23, collimation Glass tubing permanent seat 20 afterbody is inserted in the stepped hole 24 adaptive with it of housing 8 top, collimation Glass tubing permanent seat 20 afterbody lower end high-temp glue is stained with collimation Glass tubing 15, collimation Glass tubing 15 internal diameter is suitable with glass capillary 18 external diameter that need plate carbon film, collimation Glass tubing 15 is used for fixing glass capillary 18, collimation Glass tubing permanent seat 20 head is set with intermediate sleeve 13, rubber cradle 16 is provided with between intermediate sleeve 13 and collimation Glass tubing permanent seat 20 head, fastening nut 12 is sleeved on and compresses intermediate sleeve 13 with the thread fit on housing 8 outside intermediate sleeve 13 and realize hermetic seal.Rubber cradle 16 central authorities have diameter to be slightly less than the through hole of fibre diameter.The positioning convex 17 intermediate sleeve 13 is provided with on vertical chute and collimation Glass tubing permanent seat 20 coordinates, and the effect of positioning convex 17 makes intermediate sleeve 13 and collimation Glass tubing permanent seat 20 keep circumference location.The model of described CO 2 laser marking machine 1 is the CO that big nation of Shenzhen laser is produced 2-H30.Glass capillary 18 is quartz wool thin glass tube.
Embodiment 2:
The present embodiment and embodiment 1 something in common repeat no more, and difference is that it is a kind of technique of glass capillary plated surface carbon film, and it use the glass capillary surface-coated carbon film device described in embodiment 1, it comprises the steps:
(1) glass capillary plated surface carbon film device is put up, housing 8 is fixed on position mobile platform 7, rubber cradle 16 is put between intermediate sleeve 13 and collimation Glass tubing permanent seat 20, by the collimation Glass tubing 15 needing the glass capillary 18 plating carbon film to be placed in fiber clamp 14 bottom, tail optical fiber 19 is through rubber cradle 16, tighten fastening nut 12, compress intermediate sleeve 13 and rubber cradle 16, marked by the relative position of intermediate sleeve 13 with housing 8, vacuum pump 3 is connected with housing 8 by turriform joint with acetylene nitrogen gas tank 4.
(2) go out distance between luminous point and prism 2 and the prism 2 of regulation of carbon dioxide laser marking machine 1 are 22cm to the focal length that the distance sum of glass capillary 18 is CO 2 laser marking machine 1, then carried out the fine setting of distance by position mobile platform 7, stop regulating when fine setting is maximum to the brightness being observed glass capillary 18 by view port 6.
(3) open vacuum pump 3 to bleed, bleed about 5 minutes, vacuum pump 3 switch is closed when tensimeter is shown as zero, open acetylene nitrogen gas tank 4 switch, pass into reactant gases, ventilate after about 3 minutes, open vacuum pump 3 switch limit to pass into reactant gases limit and bleed, to guarantee to be full of reactant gases in housing, there is no air, then vacuum pump 3 cuts out.
(4) control software design of CO 2 laser marking machine 1 is opened, drawing mark figure is rectangle, length is about 5cm, when regulation of carbon dioxide laser marking machine 1 mark intensity is about 300bit, start to carry out mark, namely carbon dioxide laser is to the heating of glass capillary 18, because marking image is rectangle, laser can carry out mark to the total length of glass capillary 18, avoids the heating that when also needing glass capillary 18 is moved up and down when adopting the heating of laser apparatus single-point laser, disalignment causes uneven; While mark heating, reactant gases decomposes, and carbon film is deposited on the surface of glass capillary 18, to glass capillary 18 mark 2 ~ 3 times, stops mark.
(5) positioning convex 17 intermediate sleeve 13 is provided with on vertical chute and collimation Glass tubing permanent seat 20 coordinates, and the effect of positioning convex 17 makes intermediate sleeve 13 and collimation Glass tubing permanent seat 20 keep circumference location.
(6) be labeled as basis with the relative position of intermediate sleeve 13 and housing 8, with spanner, intermediate sleeve 13 is rotated clockwise 180 °, carry out local heating plating carbon film to the other one side of glass capillary 18, method is the same.
(7) after glass capillary 18 both sides carbon film has deposited, first vacuum pump 3 is opened and the acetylene reaction gas in housing 8 is extracted out, then fastening nut 12 is turned on, fiber clamp 14 is taken out, taken out from collimation Glass tubing 15 by the glass capillary 18 of plating carbon film, so far glass capillary 18 plated surface carbon film completes.
The model of CO 2 laser marking machine 1 described in the present embodiment is the CO that big nation of Shenzhen laser is produced 2-H30.Glass capillary 18 is quartz wool thin glass tube.

Claims (8)

1. a glass capillary plated surface carbon film device, it comprises the CO 2 laser marking machine be fixed on base, the prism coordinated with CO 2 laser marking machine, also comprise the housing of a hollow, housing side is provided with the optical transmission window corresponding with prism, housing is provided with the first pore and the second pore, and the first pore is communicated with vacuum pump, and the second pore is communicated with acetylene nitrogen gas tank; Housing is provided with fiber clamp, enclosure interior and hull outside hermetic seal.
2. glass capillary plated surface carbon film device according to claim 1, is characterized in that described optical transmission window adopts zinc selenide diaphragm.
3. glass capillary plated surface carbon film device according to claim 1, is characterized in that vacuum pump is connected with housing by turriform joint; Acetylene nitrogen gas tank is also connected with housing by a turriform joint.
4. glass capillary plated surface carbon film device according to claim 1, it is characterized in that being provided with view port on housing, the eyeglass on view port is fixed on housing by high-temp glue.
5. glass capillary plated surface carbon film device according to claim 1, is characterized in that case top is provided with vent valve and tensimeter.
6. glass capillary plated surface carbon film device according to claim 1, is characterized in that housing is connected with base by position mobile platform, and position mobile platform can carry out upper and lower, that front, rear, left and right are sextuple mobile fine setting relative to base.
7. glass capillary plated surface carbon film device according to claim 1, it is characterized in that fiber clamp comprises collimation Glass tubing permanent seat, collimation Glass tubing permanent seat comprises head, neck and afterbody, recess diameter is greater than head and afterbody, the head and afterbody side that collimate Glass tubing permanent seat are provided with sealing-ring, collimation Glass tubing permanent seat afterbody is inserted in case top stepped hole adaptive with it, collimation Glass tubing permanent seat afterbody lower end high-temp glue is stained with collimation Glass tubing, collimation Glass tubing internal diameter is suitable with the quartz wool thin glass tube external diameter that need plate carbon film, collimation Glass tubing is used for fixing quartz wool thin glass tube, collimation Glass tubing permanent seat head is set with intermediate sleeve, between intermediate sleeve and collimation Glass tubing permanent seat head, be provided with rubber cradle, and fastening nut is sleeved on and compresses intermediate sleeve with the thread fit on housing outside intermediate sleeve and realize hermetic seal.
8. glass capillary plated surface carbon film device according to claim 7, is characterized in that positioning convex intermediate sleeve is provided with on vertical chute and collimation Glass tubing permanent seat is slided and joins.
CN201410470320.3A 2014-09-16 2014-09-16 Glass capillary plated surface carbon film device Active CN104195527B (en)

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CN201510331571.8A CN104947066B (en) 2014-09-16 2014-09-16 Capillary glass pipe surface plates carbon technology
CN201410470320.3A CN104195527B (en) 2014-09-16 2014-09-16 Glass capillary plated surface carbon film device

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CN108468037B (en) * 2018-02-26 2019-03-29 武汉大学 Femtosecond laser predissociation device and chemical vapor depsotition equipment
CN108508531B (en) * 2018-03-22 2021-12-21 中国人民解放军国防科技大学 Capillary glass tube heating and air suction device
CN108861748B (en) * 2018-07-13 2024-01-02 江苏海狮机械股份有限公司 Spreading conveying device in spreading machine
CN112146956B (en) * 2020-09-24 2023-06-20 中国科学院重庆绿色智能技术研究院 Glass needle tip nano-hole filling device based on vacuum method and using method thereof
CN115259684B (en) * 2022-08-02 2024-03-08 安徽光智科技有限公司 Carbon plating method for quartz device

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