CN106094065B - A kind of preparation method of graded index quartz glass lens - Google Patents

A kind of preparation method of graded index quartz glass lens Download PDF

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CN106094065B
CN106094065B CN201610404370.0A CN201610404370A CN106094065B CN 106094065 B CN106094065 B CN 106094065B CN 201610404370 A CN201610404370 A CN 201610404370A CN 106094065 B CN106094065 B CN 106094065B
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quartz glass
graded index
index
lens
collapsing
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CN106094065A (en
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毛召召
熊良明
罗杰
郭飞
郭王欢
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Yangtze Optical Fibre and Cable Co Ltd
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B3/00—Simple or compound lenses
    • G02B3/0087—Simple or compound lenses with index gradient
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B33/00—Severing cooled glass
    • C03B33/06—Cutting or splitting glass tubes, rods, or hollow products
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2201/00—Glass compositions
    • C03C2201/02—Pure silica glass, e.g. pure fused quartz
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2203/00—Production processes
    • C03C2203/40—Gas-phase processes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2203/00—Production processes
    • C03C2203/50—After-treatment

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  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Surface Treatment Of Glass (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)

Abstract

The invention belongs to field of optical device technology, disclose a kind of manufacturing method of graded index (GRIN) quartz glass lens, and graded index profile includes the radially continuous reduction of refractive index and two classes of radially continuous increase.Using plasma chemical vapour deposition technique (PCVD) of the present invention deposits the quartz glass layer of doping inside bushing pipe, and control doping Ge, F, P, B content realize the consecutive variations of refractive index.Collapsing into solid GRIN sticks 10~50mm of diameter, compared with pure quartz, refractive index ndDifference is up to ± 0.08.Disc-shaped is slit longitudinally into, polishing obtains large scale graded index glass lens.Large-sized GRIN sticks are drawn into the thin GRIN sticks of 0.1~10mm of diameter under high temperature, cutting and polishing can obtain the smaller graded index glass lens of size.The present invention provides the graded index quartz glass lens that a kind of size range is wide, index distribution is arbitrarily controllable and the process routes for preparing the lens.

Description

A kind of preparation method of graded index quartz glass lens
Technical field
The invention belongs to field of optical device technology, more particularly, to a kind of graded index quartz glass lens Preparation method.
Background technology
Graded index (GRIN) lens, refer to optical lens of the material internal refractive index along a direction consecutive variations, There are three types of graded index profile types：Radial gradient index, axial gradient index, spherical surface graded index.Radially ladder It is most wide, of greatest concern to spend index lens application range, the wherein radially continuous reduction of refractive index, and light can be converged as a bit Be known as GRIN Lens；The radially continuous increase of refractive index, that disperse function is played to light is known as self-defocusing lens.Self-focusing and Such as Fig. 1 and Fig. 2, light are gradually converging or diverging with self-defocusing lens light path schematic diagram wherein respectively.Gradient-index lens have There are the characteristics such as collimation, focusing, diverging, coupling and imaging, and monochromatic aberration can be effectively reduced, including spherical aberration, aberration, distortion, field Bent and astigmatism, in addition the sShape features that its column is compact, more convenient in a variety of different micro-optics systems can make With.Gradient-index lens are essential basic devices in optical communication passive device, and for example micro- in integrated optics field The equipment such as type optical system, collimator, laser, photoswitch, medical optical instrument, optics duplicator, facsimile machine, scanner have It and is widely applied.
Lens mainly have two major class of glass and plastics by material classification.Glass lens be easy to molding, light weight, it is at low cost and It using extensive, but is influenced by the congenital fatal defects of plastic material, such as thermal expansion, hygroscopic, not organic solvent-resistant, optical system Number narrow range and easy the shortcomings of varying with temperature, still it is difficult to the application for replacing glass lens in optical articles.Optical glass by Characteristic in terms of its excellent light transmission and thermal expansion, refractive index, leading position is still occupied in high-level product. With the development of precision optical system, graded index glass applications are also increasingly wider, and optical system is to graded index glass Index distribution and glass quality made higher requirement.
From the point of view of the distribution about graded index glass lens, more is in light device based on gradient-index lens Application start in part, and lens technology of preparing and few, it is seen that gradient-index lens application is wide and effectively prepares hand Section is few.The common method for preparing graded index glass lens includes：Ion-exchange, sol-gal process, neutron irradiation method, body Diffusion method and chemical vapor deposition etc..
Ion-exchange process is the method for being used for preparing graded index glass earliest, is made using concentration of metal ions difference Diffusivity under, Ion transfer form graded index profile.There are two types of modes for ion exchange：(1) ion in melt is handed over It changes.Melten glass fiber elongation method is a kind of one-time formed technique, after the glass metal clarification homogenizing of melting, is squeezed out from below, Cheng Yi Determine the glass bar of diameter, in order to obtain graded index, another component glass metal of certain depth injection, warp at glass metal center After crossing certain ion diffusion, extrusion molding from below.A kind of double-deck melt structure is described in patent CN1495139A, is passed through The method that ion diffusion obtains gradient index rod-shape lens.This method ion free diffusing forms graded index, it is difficult to control And pollution is also easy to produce, when being squeezed out from jet hole, devitrification easily occurs, therefore yield rate is relatively low, can not prepare in addition substantially Product original paper, complex procedures, cost of manufacture are high, it is clear that cannot meet the requirement to Gradient index optics glass properties, yield. (2) ion exchange under solid-state.Diameter 1.8mm is placed on nitric acid mixed with the glass bar of thallium element in patent US6845634B2 In the salt bath of potassium, 560 DEG C heat 68~72 hours, ion exchange and form Parabolic index distribution.This method sample There must be smaller size, can be only achieved certain ion diffusion depth, the cost time is long, and yield rate is low, refractive index point The control ability of cloth is limited.
Sol-gal process is allowed to drying and sintering after forming gel and graded index glass is made using metal alkoxide as raw material Body, but vitreum prepared by the method is more crisp, transparency is poor, and the production cycle is long.Body diffusion method is by the glass of different refractivity Glass block, is placed by index distribution, and makes interface fusion under certain heat treatment condition, to obtain graded index profile. The method can obtain large-size components, and initial index of refraction distribution is easily controllable, but can only prepare axial gradient index lens, no Radial refractive index distribution can be designed.
Chemical vapor deposition is reflected using deposit glass in pipe or on substrate, control material concentration is chemically reacted with controlling Rate is distributed, and method control is accurate, but operating difficulties, and production temperature is high, the period is long.
Patent TW200641403A describes a kind of ion implantation, using lens as matrix, metal simple-substance under the electric field from Sonization accelerates into lens, forms ion concentration gradient distribution, obtains gradient-index lens.The method can be directly in lens Graded index is formed, control is more accurate, but refractive index can only be axially distributed, and depth is shallower, and high energy ionising pair sets It is standby more demanding.Patent US005630857A describes a kind of method that multilayer different densities glass melt stacks, and high density melts Body in lower section, topple over thereon successively by low-density melt, and it is poor to obtain graded index by density contrast.This method is suitable only for direction Graded index glass, and process is more difficult to control, individual layer refractive index is unevenly distributed.
In conclusion there are still more problems for existing graded index glass lens technology of preparing, rolled over including difficult to realize The accurate control of the radially uniform variation of rate is penetrated, is only capable of reaching unilateral or longitudinal refractive index distribution compared with Alternative, it is impossible to realize refraction The circle of rate is symmetrical.The ion-exchange process of mainstream, during ion exchange, control temperature, time and ion concentration, The parameters such as electric field, radial refractive index distribution is based on parabola shaped, and index distribution type is limited, and ion-exchange time is long, only It works when sample size is smaller, preparing large scale lens has very big limitation, and the heavy metal components such as Pb, Tl in glass It is harmful.
Invention content
For problems of the prior art, the present invention provides a kind of preparation side of graded index quartz glass lens Method can prepare the quartz glass lens reduced including radial refractive index gradual change and the increased quartz glass of radial refractive index gradual change Lens.
Main Control Elements in graded index glass lens manufacturing process are：Index distribution uniformity and glass object Matter.More above-mentioned several method, chemical vapor deposition are undoubtedly a kind of method that refractive index accurately controls, the present invention using etc. from Daughter chemical vapor deposition (Plasma Chemical Vapor Deposition, PCVD) method sedimentation gradient refractive index quartz Glass, furnace body temperature is lower in this method, and energy consumption can be saved compared to other methods.In the method for the present invention, what microwave cavity generated High-frequency microwave makes O2Ionization forms plasma, raw molecule dissociation ionization by electron collision, and reactive deposition is in bushing pipe Wall.As resonator is periodically axially moved, Ge, F, P, B element content in raw material are controlled, deposits from level to level that refractive index is gradually The glassy layer of change, so as to fulfill refractive index radially symmetrical uniform gradient distribution.The solid GRIN sticks that collapsing obtains, crackle, The defects of bubble, is few, and lens quality is high.The degree that sedimentation time and glass bar is controlled to draw and attenuate can obtain the cylinder of different-diameter Shape GRIN sticks, direct slicing can prepare various sizes of graded index glass lens.The technological process directly obtains use The lens of required diameter, then different thickness is cut into, simple processing is efficient.
Preparation method of the present invention mainly includes six parts：Deposition, collapsing, burn into draw and attenuate, cut and polish, specifically：
(1) it deposits：Gas raw material is transported into PCVD quartz liners, 20~100mm of bushing pipe outer diameter.Microwave resonance intracavitary Cause O2Ionization, the depositing glass layers at a temperature of 900~1500 DEG C control Ge, F, P, B element content to obtain consecutive variations Index distribution.For quartz glass, Ge is the ingredient for improving refractive index, and F, P, B can then reduce refractive index.Initial F, P, B The more Ge constituent contents of constituent content are few, as deposition carries out F, P, B element content gradually decreases Ge constituent contents and gradually increases, most Refractive index of the centre height, the index distribution that radial refractive index continuously decreases can be formed eventually.Conversely, refractive index is low centered on then, diameter The index distribution gradually risen to refractive index.
Above-mentioned offer Ge, F, P, B element ingredient can be GeCl4、PCl3、POCl3、PF3、BCl3、BF3、C2F6、CF4、 SF6.Consider for materials safety, BF3、PCl3、PF3It not uses, with SiCl4Mass content is a unit, and other components contain Amount is respectively：GeCl4：0~50%, POCl3：0~10%, BCl3：0~10%, C2F6+CF4+SF6：0~40%, O2：100% ~200%.Sedimentation time 6~20 hours, totally 1000~100000 layers of the deposit glass number of plies, the μ of thickness in monolayer range 10nm~10 m.Raw material is formed to be represented between refractive index value by formula, inclined between actual test refractive index value and setting value by correcting Difference adjusts component ratio so that actual refractive index is more bordering on setting value.
(2) collapsing：Bushing pipe center can not be deposited to closed state, and bushing pipe is transferred to collapsing stove collapsing, 1500~ Under 2500 DEG C of high temperature, certain negative pressure is kept inside pipe, glass tube is made to generate contraction under the action of inside and outside differential pressure and surface tension, Bushing pipe internal diameter is gradually reduced to completely disappearing to obtain GRIN sticks.During collapsing, interlayer ion is spread so that refractive index more becomes In continuous gradation.During collapsing, bushing pipe does not stop to rotate, and bushing pipe during softening is prevented to be bent, 10~100r/min of speed melts After the completion of contracting, 10~50mm of GRIN stick diameters.
Fig. 3 is GRIN stick radial refractive index distribution schematic diagrames, and equation is：
In formula, n0：Represent the refractive index of the centre of GRIN Lens
r：Represent the radius of GRIN Lens
Represent the index distribution constant of GRIN Lens
In index distribution general formula, i=2, k1=0, k2=-A/2, refractive index are parabola shaped distribution.
(3) corrode：It is carried out since PCVD is deposited on inside bushing pipe, so after collapsing, outermost layer is nonspecific cellular immunity area Domain can play a protective role to center effective coverage, avoid chemically or physically damaging.Refraction index test can determine GRIN stick cores Covering size according to actual demand erodable section outer surface or can not corrode, to obtain suitable core packet ratio.
(4) it draws and attenuates：By GRIN sticks vertically depending in high temperature furnace, 1000~2200 DEG C of the temperature in lower section in stove, glass is gradual It is flowed down after melting, by 800~1200 DEG C of holding furnaces, controls certain drop-down speed and the amount of feeding, can accurately regulate and control GRIN Stick diameter, drawing diameter is smaller, and draw rate is faster, and prestissimo can reach 2000m/min, 0.1~10mm of diameter after drawing-down, The stub that GRIN sticks are truncated into 0.1~3m length is collected.With pure quartzy refractive indexIt compares, largest refractive index difference Δ n It is ± 0.08, variations in refractive index section is It is up to 0.535.
(5) it cuts：The GRIN sticks for not drawing and having drawn radially are cut, the GRIN sticks of different-diameter are cut into The pre-shaped lens of different length.Center and one timing of outer layer refringence, diameter is smaller, and refractive index curvature is bigger, refractive power effect It is more notable, relatively short length is needed to realize the convergence and diverging of light.According to actual refractive index distribution come Cutting Length, preferably 1~50mm of length range.
For the self-focusing quartz lens of parabola shaped index distribution, according to the use demand under different wave length, cutting Into different length.Test, with radius distribution curve, calculates refractive index gradient constant using the refractive index under wavelength" section Away from " P refers to and account for light and propagate sine wave period numerical value, generally 1/4 cycle in lens, i.e., directional light is for the first time and optical axis It is intersecting, also according to length of lens or 1/4+n/2 sine wave period.According to " pitch " set, calculated by following formula Length needed for lens：
Equally, the focal length of lens can also be calculated：
(6) it polishes：The outer layer that light region does not include bushing pipe collapsing and forms is passed since grin lens are practical, outer layer can play Protective effect, GRIN sticks side surface has been smooth minute surface, does not need to do multiprocessing, the columnar pre-shaped lens cut into Afterwards, it needs to handle cutting section, cutting polishing obtains planar lens, spherical lens or non-spherical lens.
Fig. 4 is a kind of GRIN Lens schematic diagram of parabola shaped index distribution, on radial section at central shaft distance r Refractive index is circularly symmetric, and parallel incoming rays are in center convergence.General GRIN Lens based on the borosilicate of multicomponent mixture, Main cause is that such glass formation temperature is low, easily prepared, especially for ion-exchange, ion-exchange time under high temperature It is long, sample is needed to have relatively low softening temperature, ion could preferably move to form refringence.And quartz glass Melting temperature is high, it is clear that ion-exchange is not suitable for preparing the gradient-index lens of quartz glass material.But meanwhile quartz Optical glass compares the optical glass of general component, there is great advantage, has better light transmittance, has better resistance to height Warm nature energy, hardness is high, wear-resisting, corrosion-resistant, resistance to heat shocks, there is smaller coefficient of thermal expansion, in optic communication 1310nm, 1550nm Have lower attenuation coefficient in wave band, under harsh occasion, quartz glass be obtain high stable optical parameter must can not Few material.
The present invention has following several respects to innovate：
For these problems and the unique advantage of quartz glass, the present invention proposes a kind of graded index of quartz material The preparation method of glass lens can obtain the quartz glass lens of a wide range of sizes of 0.1~50mm of diameter, lens sizes range Far super general gradient-index lens.Doped chemical is free of the harmful heavy metal ions such as thallium, lead, and preparation time is relatively short, and Single output is big, greatly improves the efficiency.Collapsing and drawing can prepare cylindric glass, directly radially be sliced, cross section Polishing can obtain gradient-index lens, and processing is simple.
Most important, common ion-exchange, by the way that extraneous ion concentration, heating temperature, time etc. is controlled to join indirectly Number control ion diffusion profile, artificial is difficult accurate regulation and control refractive index, and practical index distribution often deviates perfect condition, special Not lens edge, deviation is larger, refractive index generally with radially show as near parabolic shape distribution.And PCVD methods can be accurate Control nanometer grade thickness glassy layer doped chemical content, means are more direct, and as needed, can realize trigonometric function type, The index distribution that linear type, parabolic type, cubic curve type or other high order curve types or a variety of curve combinations form, always It, in our the attainable index regions of institute, can realize required Arbitrary index profiles.Such as Fig. 5 index distributions In schematic diagram, 1 is parabola shaped index distribution, and 2 be linear distribution.
Description of the drawings
Fig. 1 is directional light incidence self-focusing glass lens light path schematic diagram；
Fig. 2 is directional light incidence self-defocusing glass lens light path schematic diagram；
Fig. 3 is GRIN stick radial refractive index distribution schematic diagrames in the embodiment of the present invention；
Fig. 4 is a kind of gradient-index lens and index distribution schematic diagram；
Fig. 5 is two kinds of radial refractive index distribution schematic diagram；
Fig. 6 is the self-focusing quartz glass lens refractive index profile described in the embodiment of the present invention one；
Fig. 7 is the self-defocusing quartz glass lens refractive index profile described in the embodiment of the present invention three.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below It does not constitute a conflict with each other and can be combined with each other.
Embodiment one
(1) the quartz glass bushing pipe of diameter 31mm, thick 2mm in PCVD equipment, are passed through SiCl4、C2F6、GeCl4、 O2Gas, 1100 DEG C of furnace body heating temperature start to deposit, initial C under high-frequency microwave effect2F6Content is in maximum value, GeCl4Content is in minimum value, subsequent C2F6Dosage continuously decreases, GeCl4Dosage gradually rises, certain phase C2F60 is reduced to, after It is continuous to be passed through GeCl4Deposition, overall process deposit 8 hours, and PCVD terminates to complete entire deposition process automatically.
(2) after the completion of depositing, to collapsing stove, the collapsing at 2100 DEG C, bushing pipe is rotated transfer bushing pipe with 40r/min speed, Set temperature program after initially forming sealing from centre, is extended to both sides, until central duct is closed completely, collapsing is into diameter The GRIN sticks of 25mm.Horizontal region is presented as liner portion in refractive index curve such as Fig. 6, refractive index, and central area is refractive index Show as Parabolic GRIN Lens part, diameter 19mm.The initial C for being passed through more amount2F6, there are cliff of displacement formulas for refractive index It reduces, subsequent C2F6Content continuously decreases, GeCl4Content gradually increases, and parabolically type rises refractive index, and final stage is lasting Increase GeCl4Dosage further improves refractive index.Center parabola branch, refractive index are with radial distribution equation：
Wherein, n0=1.4786,
(3) GRIN sticks are corroded to diameter 21mm, obtain 0.9 core packet than GRIN sticks, clean up for draw and attenuate process do Prepare.
(4) the GRIN sticks corroded are shifted and drawn and attenuated, GRIN sticks are hung in furnace interior, furnace body lower section temperature 1800 vertically DEG C, the melting of stick lower end attenuates and falls, by 800 DEG C of holding furnaces, using cooling chamber, by control lower section apply pulling force and into The thin GRIN sticks of diameter 2mm, draw rate 50m/min are obtained to amount adjustment.After GRIN sticks draw and attenuate, reflected between center and outer layer Rate difference is basically unchanged, since diameter becomes smaller,Value increase.
(5) long thin GRIN sticks are cut into the pre-shaped lens that 2~20mm do not wait, end face is polished to parallel minute surface, as Graded index self-focusing glass lens.
Embodiment two
(1) the quartz glass bushing pipe of diameter 35mm, thick 3mm in PCVD equipment, are passed through SiCl4、C2F6、SF6、O2 Gas, 1100 DEG C of furnace body heating temperature start to deposit under high-frequency microwave effect, generation F doping SiO2, reduce refractive index.Most Just it is passed through a small amount of C2F6+SF6, buffer layer, after a period of time, by C2F6+SF6Dosage is adjusted to maximum, subsequent C2F6+SF6Contain Amount continuously decreases, GeCl4Content gradually increases, and deposits 8 hours, completes entire deposition process.
(2) after the completion of depositing, to collapsing stove, the collapsing at 2100 DEG C, bushing pipe is rotated transfer bushing pipe with 60r/min speed, Set temperature program after initially forming sealing from centre, is extended to both sides, until central duct is closed completely, collapsing is into diameter The GRIN sticks of 30mm.
(3) by the GRIN sticks cut into 10~50mm of length not wait pre-shaped lens, end face is polished to minute surface, as Φ 30 Large-sized graded index self-focusing glass lens.Center parabolic type region is qualified graded index region, Peripheral part can be cut away, and can also be used as lens packages region, be played the role of fixed.
Embodiment three
(1) the quartz glass bushing pipe of diameter 50mm, thick 4mm in PCVD equipment, are passed through SiCl4、GeCl4、O2Gas Body, 1200 DEG C of furnace body heating temperature start to deposit under high-frequency microwave effect, generation Ge doping SiO2, initially it is passed through GeCl4Contain Amount gradually increases, and refractive index improves.After depositing 2 hours, GeCl4When dosage is to certain value, and continuously decrease, at the same time by Gradually add C2F6+CF4+POCl3, 8 hours of subsequent deposition time, final GeCl4Dosage is to minimum, C2F6+CF4+POCl3With Maximum value is measured, terminates entire deposition process, total 10 hours of sedimentation time.
(2) after the completion of depositing, to collapsing stove, the collapsing at 2000 DEG C, bushing pipe is rotated transfer bushing pipe with 40r/min speed, Set temperature program after initially forming sealing from centre, is extended to both sides, until central duct is closed completely, collapsing is into diameter The GRIN sticks of 27mm.Refractive index curve such as Fig. 7, refractive index show as Parabolic central area as self-defocusing lens component, Diameter 20mm.Initial GeCl4Content gradually rises, and refractive index rises, its subsequent content declines, and F, P element content increase, folding There is parabolic type reduction in the rate of penetrating.
Wherein, n0=1.4355,
(3) GRIN sticks are corroded to diameter 25mm, obtain 0.8 core packet than GRIN sticks, clean up for draw and attenuate process do Prepare.
(4) the good GRIN sticks of collapsing are shifted and drawn and attenuated, it is hung in furnace interior vertically, 1900 DEG C of the temperature in furnace body lower section, The melting of stick lower end attenuates and falls, by 800 DEG C of holding furnaces, using cooling chamber, by the way that lower section is controlled to apply pulling force and feeding Amount adjustment obtains the thin GRIN sticks of diameter 2mm, draw rate 50m/min.After GRIN sticks draw and attenuate, refractive index between center and outer layer Difference is basically unchanged, since diameter becomes smaller,Value increase.
(5) by long thin GRIN sticks cut into 2~20mm not wait pre-shaped lens, a side end face is polished to vertical center axis Minute surface, opposite side is polished to and 8 ° of angle mirror faces of central shaft, as graded index self-defocusing glass lens.
Example IV
(1) the quartz glass bushing pipe of diameter 45mm, thick 4mm in PCVD equipment, are passed through SiCl4、GeCl4、O2Gas Body, 1200 DEG C of furnace body heating temperature start to deposit under high-frequency microwave effect, generation Ge doping SiO2, improve refractive index.Initially GeCl4Content is gradually risen to certain value, after continuously decrease, at the same time gradually add C2F6+CF4+BCl3, 8 hours are deposited, Complete entire deposition process.
(2) after the completion of depositing, to collapsing stove, the collapsing at 2000 DEG C, bushing pipe is rotated transfer bushing pipe with 60r/min speed, Set temperature program after initially forming sealing from centre, is extended to both sides, until central duct is closed completely, collapsing is into diameter The GRIN sticks of 30mm.
(3) directly by the GRIN sticks cut into 10~50mm not wait pre-shaped lens, end face is polished to minute surface, as gradient Refractive index self-defocusing glass lens.Center parabolic type region is qualified graded index region, and peripheral part can be with It cuts away, can also be used as lens packages region, play the role of fixed.
It is apparent that the present invention manufactures graded index glass lens using PCVD methods, can freely be accurately controlled Index distribution, refractive index are centrosymmetric distribution, and different size lens in preferable cylindric, only do briefly by above example Explanation.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to The limitation present invention, all any modification, equivalent and improvement made all within the spirits and principles of the present invention etc., should all include Within protection scope of the present invention.

Claims (7)

  1. A kind of 1. preparation method of graded index quartz glass lens, which is characterized in that using plasma chemical vapor deposition Product deposits the quartz glass layer of doping inside glass bushing pipe, then collapsing is and straight into solid gradient index rod in collapsing stove It connects slice or is sliced after being drawn into thin gradient index rod, be finally polished to lens, wherein：
    Totally 1000~100000 layers of the quartz glass layer of deposition, layer thickness ranging from 10nm~10 μm；
    1500~2500 DEG C of collapsing temperature, barred body axial-rotation 10~100r/min of frequency, a diameter of 10~50mm after collapsing；
    The raw material of plasma activated chemical vapour deposition is, with SiCl4Mass content is a unit, and other components content is respectively： GeCl4：0~50%, POCl3：0~10%, BCl3：0~10%, C2F6+CF4+SF6：0~40%, O2：100%~200%.
  2. 2. the preparation method of graded index quartz glass lens according to claim 1, which is characterized in that the bushing pipe Material is quartz, and outer diameter is 20~100mm, and thickness is 2~20mm.
  3. 3. the preparation method of graded index quartz glass lens according to claim 1 or 2, which is characterized in that wait from The microwave frequency of daughter chemical vapor deposition is 2.45GHz, and depositing temperature is 900~1500 DEG C.
  4. 4. the preparation method of graded index quartz glass lens according to claim 1 or 2, which is characterized in that heavy During product GRIN Lens, P, B, F constituent content are high in initial feed, then continuously decrease, Ge constituent contents gradually rise；Heavy During product self-defocusing lens, Ge constituent contents are high in initial feed, then continuously decrease, P, B, F constituent content gradually rise.
  5. 5. the preparation method of graded index quartz glass lens according to claim 1 or 2, which is characterized in that described Collapsing continuously draws and attenuates vertically into solid gradient index rod, gradient index rod in collapsing stove, the graded index after drawing-down Stick diameter range is 0.1~10mm.
  6. 6. the preparation method of graded index quartz glass lens according to claim 5, which is characterized in that in collapsing stove During middle collapsing, it is 1600~2200 DEG C to heat and soften temperature range, gradient index rod annealing region after drawing-down It is 800~1200 DEG C.
  7. 7. the preparation method of graded index quartz glass lens according to claim 1 or 2, which is characterized in that polishing The surface roughness Ra of graded index quartz glass lens afterwards<5nm.
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CN113391383B (en) * 2021-06-09 2022-11-08 上海大学 Preparation method for printing ultramicro-lens with periodic micro-nano structure gradient refractive index by adopting grid electrode micro-thermal polarization
CN115220135A (en) * 2022-08-05 2022-10-21 上海中科澳谱光电器件有限公司 Spherical micro self-focusing lens and production method thereof

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