CN106094065A - 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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Publication number
CN106094065A
CN106094065A CN201610404370.0A CN201610404370A CN106094065A CN 106094065 A CN106094065 A CN 106094065A CN 201610404370 A CN201610404370 A CN 201610404370A CN 106094065 A CN106094065 A CN 106094065A
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quartz glass
graded index
glass lens
index
preparation
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CN106094065B (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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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

Abstract

The invention belongs to field of optical device technology, disclose the manufacture method of a kind of graded index (GRIN) quartz glass lens, graded index profile includes that refractive index is radially continuous and reduces and radially continuous increase two classes.The quartz glass layer that using plasma chemical vapour deposition technique (PCVD) of the present invention is adulterated in bushing pipe inside deposition, control doping Ge, F, P, B content realize the consecutive variations of refractive index.Solid GRIN rod diameter 10～50mm that collapsing becomes, compared with pure quartz, refractive index ndDifference is ± 0.08 to the maximum.Slitting longitudinally into disc-shaped, polishing obtains large scale graded index glass lens.Large-sized GRIN rod is drawn under high temperature diameter 0.1～10mm thin GRIN rod, and cutting and polishing can obtain the less graded index glass lens of size.The invention provides the graded index quartz glass lens that a kind of size range is wide, index distribution is arbitrarily controlled, and prepare the process route of this 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 material internal refractive index along a direction continually varying optical lens, Graded index profile type has three kinds: radial gradient index, axial gradient index, sphere graded index.Radially ladder Degree index lens range of application is the widest, of greatest concern, and the wherein radially continuous reduction of refractive index, and light can be converged as a bit Be referred to as GRIN Lens；The radially continuous increase of refractive index, that plays disperse function to light is referred to as self-defocusing lens.Self-focusing and Self-defocusing lens light path schematic diagram is respectively such as Fig. 1 and Fig. 2, and light is progressively converging or diverging with wherein.Gradient-index lens has There is collimation, focus on, dissipate, couple and the characteristic such as imaging, and can effectively reduce monochromatic aberration, including spherical aberration, aberration, distortion, field Bent and astigmatism, adds the small and exquisite profile feature of its column, can convenient making in multiple different micro-optics systems With.Gradient-index lens is requisite basic device in optical communication passive device, and for example micro-in integrated optics field The equipment such as type optical system, collimater, laser instrument, photoswitch, medical optical instrument, optics duplicator, facsimile machine, scanner have And be widely applied.
Lens mainly have glass and the big class of plastics two by material classification.Glass lens be easy to shaping, light weight, low cost and Use extensively, but affected by the congenital fatal defects of plastic material, such as thermal expansion, hygroscopic, not organic solvent-resistant, optical system Number narrow range and the shortcoming such as easily vary with temperature, are still difficult to replace application in optical articles for the glass lens.Optical glass by Characteristic in terms of its excellent light transmission and thermal expansion, refractive index, still occupies leading position in high-level product. With the development of precision optical system, graded index glass applications is also increasingly wider, and optical system is to graded index glass Index distribution and glass quality be proposed higher requirement.
From the point of view of the distribution with regard to graded index glass lens, more is at light device based on gradient-index lens Application start in part, and lens technology of preparing is simultaneously few, it is seen that hand extensively and is effectively prepared in gradient-index lens application Section is few.The common method preparing graded index glass lens includes: ion-exchange, sol-gal process, neutron irradiation method, body Diffusion method and chemical gaseous phase deposition etc..
Ion-exchange process is the method for preparing graded index glass the earliest, utilizes concentration of metal ions difference to make Diffusivity under with, Ion transfer forms graded index profile.Ion exchange has two ways: the ion in (1) melt is handed over Change.Melten glass fiber elongation method is a kind of one-time formed technique, after melted glass metal clarification homogenizing, extrudes from below, Cheng Yi Determine the glass bar of diameter, in order to obtain graded index, inject another kind of component glass metal, warp at glass metal center certain depth After crossing certain ion diffusion, extrusion molding from below.Patent CN1495139A describes a kind of double-deck melt structure, passes through Ion diffusion obtains the method for gradient index rod-shape lens.This method ion free diffusing forms graded index, is difficult to control And it is easily generated pollution, and it when jet hole is extruded, is susceptible to devitrification, therefore yield rate is relatively low, cannot prepare substantially in addition Long-pending original paper, complex procedures, cost of manufacture are high, it is clear that can not meet the requirement to Gradient index optics glass properties, yield. (2) the ion exchange under solid-state.It by diameter 1.8mm mixed with the glass bar of thallium element in patent US6845634B2, is placed on nitric acid In the salt bath of potassium, 560 DEG C are heated 68～72 hours, and ion exchanges and forms Parabolic index distribution.This method sample Must have less size, can be only achieved certain ion diffusion depth, spend the time long, yield rate is low, and refractive index is divided The control ability of cloth is limited.
Sol-gal process is with metal alkoxide as raw material, and after being allowed to form gel, drying and sintering prepares graded index glass Body, but vitreum prepared by this 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 the conditions of certain heat treatment, to obtain graded index profile. This 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 gaseous phase deposition utilizes chemical reaction in pipe or deposit glass on substrate, and control material concentration is to control refraction Rate is distributed, and the control of this method is accurate, but operating difficulties, production temperature is high, the cycle is long.
Patent TW200641403A describes a kind of ion implantation, with lens as matrix, metal simple-substance under the electric field from Sonization, accelerates into lens, forms ion concentration gradient distribution, it is thus achieved that gradient-index lens.This method can be directly in lens Forming graded index, control is more accurate, but refractive index can only be axially distributed, and the degree of depth is shallower, high energy ionising to setting Standby requirement is higher.Patent US005630857A describes the method for a kind of multilayer different densities glass melt stacking, and high density melts Body is in lower section, and low-density melt is toppled on it successively, is obtained gradient refractive index rate variance by density contrast.This method is suitable only for a direction Graded index glass, and the more difficult control of process, individual layer refractive index skewness.
In sum, existing graded index glass lens technology of preparing still suffers from more problem, including be difficult to realize folding The accurate control of the radially uniform change of rate of penetrating, 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 main flow, during ion exchange, control temperature, time and ion concentration, The parameters such as electric field, radial refractive index distribution is with based on parabola shaped, and index distribution type is limited, and ion-exchange time is long, only The onset when sample size is less, preparation large scale lens have the heavy metal component such as very big restriction, and Pb, the Tl in glass Harmful.
Content of the invention
For problems of the prior art, the present invention provides the preparation side of a kind of graded index quartz glass lens Method, can prepare and include quartz glass lens that radial refractive index gradual change reduces and the quartz glass that radial refractive index gradual change increases Lens.
Main Control Elements in graded index glass lens manufacture process is: index distribution uniformity and glass object Matter.Relatively more above-mentioned several method, chemical gaseous phase deposition is undoubtedly a kind of method that refractive index accurately controls, employing of the present invention etc. from Sub-body chemical vapor phase growing (Plasma Chemical Vapor Deposition, PCVD) method sedimentation gradient refractive index quartz Glass, in the method, furnace body temperature is lower, compares additive method and can save energy consumption.In the inventive method, microwave cavity produces High-frequency microwave makes O2Ionization forms plasma, raw molecule dissociation ionization by electron collision, and reactive deposition is in bushing pipe Wall.With the periodic axially-movable of resonator, Ge, F, P, B element content in control raw material, deposit from level to level that refractive index is gradually The glassy layer becoming, thus realize the uniform gradient distribution that refractive index is radially symmetrical.The solid GRIN rod that collapsing obtains, crackle, The defects such as bubble are few, and lens quality is high.The degree that control sedimentation time and glass bar draw and attenuate, is obtained in that the cylinder of different-diameter Shape GRIN rod, direct slicing can prepare various sizes of graded index glass lens.This technological process directly obtains use The lens of required diameter, then cut into different thickness, processing simplicity, efficiency is high.
Preparation method of the present invention mainly includes six parts: deposition, collapsing, burn into draw and attenuate, cut and polishing, specifically:
(1) deposit: gas raw material is transported in PCVD quartz liner, bushing pipe external diameter 20～100mm.In microwave cavity Make O2Ionization, depositing glass layers at a temperature of 900～1500 DEG C, control Ge, F, P, B element content are to obtain continually varying Index distribution.For quartz glass, Ge is the composition improving refractive index, and F, P, B then can reduce refractive index.Initial F, P, B Constituent content many Ge constituent content is few, with deposition carry out F, P, B element content gradually decrease Ge constituent content and gradually increase, Refractive index of the centre can be formed eventually high, the index distribution that radial refractive index is gradually lowered.Otherwise, then centered on refractive index low, footpath The index distribution gradually rising to refractive index.
Above-mentioned offer Ge, F, P, the composition of B element can be GeCl4、PCl3、POCl3、PF3、BCl3、BF3、C2F6、CF4、 SF6.Consider for materials safety, BF3、PCl3、PF3Not use, with SiCl4Mass content is a unit, and other components contain Amount is respectively as follows: GeCl4: 0～50%, POCl3: 0～10%, BCl3: 0～10%, C2F6+CF4+SF6: 0～40%, O2: 100% ～200%.Sedimentation time 6～20 hours, the deposit glass number of plies totally 1000～100000 layers, thickness in monolayer scope 10nm～10 μ m.Raw material composition with refractive index value between represented by formula, by correction reality test refractive index value and setting value between inclined Difference, adjusts component ratio so that actual refractive index more levels off to setting value.
(2) bushing pipe is transferred to collapsing stove collapsing by collapsing: bushing pipe center cannot deposit to closed state, 1500～ Under 2500 DEG C of high temperature, pipe is internal keeps certain negative pressure, makes glass tube produce contraction under inside and outside differential pressure and capillary effect, Bushing pipe internal diameter be gradually reduced to be wholly absent obtain GRIN rod.During collapsing, interlayer ion diffusion makes refractive index more become In continuous gradation.During collapsing, bushing pipe does not stop to rotate, bushing pipe bending when preventing from softening, and speed 10～100r/min is molten After contracting completes, GRIN rod diameter 10～50mm.
Fig. 3 is GRIN rod radial refractive index distribution schematic diagram, and its equation is:
n ( r ) = n 0 ( 1 - ( A r ) 2 2 )
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
n ( r ) = | Σ i = 0 k i r i |
In index distribution formula, i=2, k1=0, k2=-A/2, refractive index is parabola shaped distribution.
(3) corrode: carry out owing to PCVD is deposited on inside bushing pipe, so after collapsing, outermost layer is nonspecific cellular immunity district Territory, can play a protective role to effective coverage, center, it is to avoid chemically or physically damage.Refraction index test can determine GRIN rod core Covering size, can erodable section outer surface or do not corrode, to obtain suitable core bag ratio according to the actual requirements.
(4) draw and attenuate: by GRIN rod vertically depending in high temperature furnace, lower section temperature 1000～2200 DEG C in stove, glass is gradually Flow down after Rong Rong, through 800～1200 DEG C of holding furnaces, control certain drop-down speed and the amount of feeding, can accurately regulate and control GRIN Rod diameter, draws diameter less, and draw rate is faster, and prestissimo can reach 2000m/min, diameter 0.1～10mm after drawing-down, The stub that GRIN rod is truncated into 0.1～3m length is collected.With pure quartz refractive indexCompare, largest refractive index difference Δ n For ± 0.08, variations in refractive index interval is It is 0.535 to the maximum.
(5) cut: radially cutting the GRIN rod not drawing and having drawn, the GRIN rod of different-diameter cuts into The pre-shaped lens of different length.Center and outer layer refringence one timing, diameter is less, and refractive index curvature is bigger, refractive power effect More notable, need relatively short length to realize the convergence of light and dissipate.It is distributed Cutting Length according to actual refractive index, preferably Length range 1～50mm.
For the self-focusing quartz lens of parabola shaped index distribution, according to the use demand under different wave length, cutting Become different length.Test uses the refractive index under wavelength with radius distribution curve, calculates refractive index gradient constant" joint Away from " P refers to account for light and propagate sine wave period numerical value in lens, generally 1/4 cycle, i.e. directional light are for the first time and optical axis Intersect, also according to length of lens, it is possible to be 1/4+n/2 sine wave period.According to " pitch " that set, calculated by following formula Lens Len req:
L = 2 π P A
Equally, it is also possible to the calculating focal length of lens:
f = 1 n 0 A s i n ( A L )
(6) polish: owing to grin lens actual biography light region does not comprise the outer layer of bushing pipe collapsing, outer layer can play Protective effect, GRIN rod side surface has been smooth minute surface, it is not necessary to did multiprocessing, the pre-shaped lens of the column cutting into After, needing to process cutting section, cutting polishing obtains planar lens, spherical lens or non-spherical lens.
Fig. 4 is the GRIN Lens schematic diagram of a kind of parabola shaped index distribution, on radial section at central shaft distance r Refractive index is circularly symmetric, and parallel incoming rays is at center convergence.Based on general GRIN Lens is with the borosilicate of multicomponent mixture, Main cause is that such glass formation temperature is low, it is easy to preparation, especially for ion-exchange, and ion-exchange time under high temperature Long, need sample to have relatively low softening temperature, ion could preferably move to form refringence.And quartz glass Melt 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 The optical glass of general component compared by optical glass, has great advantage, has more preferable light transmittance, has more preferable resistance to height Warm nature energy, hardness is high, wear-resisting, corrosion-resistant, resistance to heat shocks, has less thermal coefficient of expansion, at optic communication 1310nm, 1550nm Having lower attenuation coefficient in wave band, under harsh occasion, quartz glass is that acquisition high stable optical parametric must Few material.
The present invention has following several respects to innovate:
For the unique advantage of these problems and quartz glass, the present invention proposes the graded index of a kind of quartz material The preparation method of glass lens, is obtained in that the quartz glass lens of diameter 0.1～50mm size on a large scale, lens sizes scope Remote super general gradient-index lens.Doped chemical does not contains the harmful heavy metal ions such as thallium, lead, and preparation time is relatively short, and Single output is big, substantially increases efficiency.Collapsing and drawing can prepare cylindric glass, directly radially cut into slices, cross section Polishing can obtain gradient-index lens, and processing is simple.
Topmost, common ion-exchange, by the ginseng indirectly such as the extraneous ion concentration of control, heating-up temperature, time Numerical control ion diffusion profile, artificial very difficult accurately regulation and control refractive index, actual index distribution often deviates perfect condition, special Not being lens edge, deviation is relatively big, and refractive index typically shows as the distribution of near parabolic shape with radial direction.And PCVD method can be accurate Control nanometer grade thickness glassy layer doped chemical content, means are more direct, and as required, it is possible to achieve trigonometric function type, The index distribution of linear pattern, parabolic type, cubic curve type or other high order curve types or multiple curve combination, always It, the index region that can reach at us is interior, is capable of required Arbitrary index profiles.Such as Fig. 5 index distribution In schematic diagram, 1 is parabola shaped index distribution, and 2 is linear distribution.
Brief description
Fig. 1 is the incident self-focusing glass lens light path schematic diagram of directional light；
Fig. 2 is the incident self-defocusing glass lens light path schematic diagram of directional light；
Fig. 3 is GRIN rod radial refractive index distribution schematic diagram 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 index of refraction in lens distribution map described in the embodiment of the present invention one；
Fig. 7 is the self-defocusing quartz glass index of refraction in lens distribution map described in the embodiment of the present invention three.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right The present invention is further elaborated.It should be appreciated that specific embodiment described herein only in order to explaining the present invention, and It is not used in the restriction present invention.If additionally, technical characteristic involved in each embodiment of invention described below The conflict of not constituting each other just can be mutually combined.
Embodiment one
(1) the quartz glass bushing pipe of diameter 31mm, thick 2mm, it is arranged on PCVD equipment, be passed through SiCl4、C2F6、GeCl4、 O2Gas, body of heater heating-up temperature 1100 DEG C, under high-frequency microwave effect, start deposition, initial C2F6Content is in maximum, GeCl4Content is in minimum of a value, subsequently C2F6Consumption is gradually lowered, GeCl4Consumption gradually rises, certain phase C2F6Reduce to 0, continue Continue and be passed through GeCl4Deposition, overall process deposits 8 hours, and PCVD terminates to complete whole deposition process automatically.
(2) after deposition completes, transfer bushing pipe to collapsing stove, collapsing at 2100 DEG C, bushing pipe rotates with 40r/min speed, Design temperature program, after centre initially forms sealing, to both sides extension, of completely closed to central duct, collapsing becomes diameter The GRIN rod of 25mm.Refractive index curve such as Fig. 6, the region that refractive index presents level is liner portion, and central area is refractive index Show as Parabolic GRIN Lens part, diameter 19mm.It is initially passed through the C of more amount2F6, there is cliff of displacement formula in refractive index Reduce, C subsequently2F6Content is gradually lowered, GeCl4Content is gradually increased, and refractive index parabolically type rises, and final stage is lasting Strengthen GeCl4Consumption improves refractive index further.Center parabola branch, refractive index with radial distribution equation is:
n ( r ) = n 0 ( 1 - ( A r ) 2 2 )
Wherein, n0=1.4786,
(3) by GRIN rod corrosion to diameter 21mm, obtain 0.9 core bag than GRIN rod, clean up and do for drawing and attenuating operation Prepare.
(4) drawing and attenuating the GRIN rod transfer corroded, GRIN rod is vertically hung in furnace interior, temperature 1800 below body of heater DEG C, rod lower end is melted to attenuate and drops, through 800 DEG C of holding furnaces, then through cooling chamber, by applying pulling force below control and entering Adjust the thin GRIN rod obtaining diameter 2mm, draw rate 50m/min to amount.After GRIN rod draws and attenuates, reflect between center and outer layer Rate difference is basically unchanged, owing to diameter diminishes,Value increases.
(5) long thin GRIN rod cutting into the pre-shaped lens that 2～20mm does not waits, end face is polished to parallel minute surface, is Graded index self-focusing glass lens.
Embodiment two
(1) the quartz glass bushing pipe of diameter 35mm, thick 3mm, it is arranged on PCVD equipment, be passed through SiCl4、C2F6、SF6、O2 Gas, body of heater heating-up temperature 1100 DEG C, under high-frequency microwave effect, start deposition, generate F doping SiO2, reduce refractive index.? It is just passed through a small amount of C2F6+SF6, buffer layer, after a period of time, by C2F6+SF6Consumption is adjusted to maximum, subsequently C2F6+SF6Contain Amount is gradually lowered, GeCl4Content is gradually increased, and deposits 8 hours, completes whole deposition process.
(2) after deposition completes, transfer bushing pipe to collapsing stove, collapsing at 2100 DEG C, bushing pipe rotates with 60r/min speed, Design temperature program, after centre initially forms sealing, to both sides extension, of completely closed to central duct, collapsing becomes diameter The GRIN rod of 30mm.
(3) this GRIN rod cuts into the pre-shaped lens that length 10～50mm does not waits, and end face is polished to minute surface, is Φ 30 Large-sized graded index self-focusing glass lens.Parabolic type region, center is qualified graded index region, Peripheral part can cut away, it is also possible to as lens packages region, plays fixing effect.
Embodiment three
(1) the quartz glass bushing pipe of diameter 50mm, thick 4mm, it is arranged on PCVD equipment, be passed through SiCl4、GeCl4、O2Gas Body, body of heater heating-up temperature 1200 DEG C, under high-frequency microwave effect, start deposition, generate Ge doping SiO2, it is initially passed through GeCl4Contain Amount is gradually increased, and refractive index improves.After depositing 2 hours, GeCl4When consumption is to certain value, be gradually lowered again, meanwhile by Gradually add C2F6+CF4+POCl3, 8 hours of subsequent deposition time, final GeCl4Consumption is to minimum, C2F6+CF4+POCl3With Amount arrives maximum, terminates whole deposition process, 10 hours of total sedimentation time.
(2) after deposition completes, transfer bushing pipe to collapsing stove, collapsing at 2000 DEG C, bushing pipe rotates with 40r/min speed, Design temperature program, after centre initially forms sealing, to both sides extension, of completely closed to central duct, collapsing becomes diameter The GRIN rod of 27mm.Refractive index curve such as Fig. 7, it is self-defocusing lens component that refractive index shows as Parabolic central area, Diameter 20mm.Initial GeCl4Content gradually rises, and refractive index rises, and its content declines subsequently, and F, P element content increase, folding The rate of penetrating occurs that parabolic type reduces.
n ( r ) = n 0 ( 1 + ( A r ) 2 2 )
Wherein, n0=1.4355,
(3) by GRIN rod corrosion to diameter 25mm, obtain 0.8 core bag than GRIN rod, clean up and do for drawing and attenuating operation Prepare.
(4) GRIN rod transfer good for collapsing is drawn and attenuated, it is vertically hung in furnace interior, temperature 1900 DEG C below body of heater, Rod lower end is melted to attenuate and drops, and through 800 DEG C of holding furnaces, then through cooling chamber, applies pulling force and feeding by below control Amount adjusts the thin GRIN rod obtaining diameter 2mm, draw rate 50m/min.After GRIN rod draws and attenuates, refractive index between center and outer layer Difference is basically unchanged, owing to diameter diminishes,Value increases.
(5) long thin GRIN rod cutting into the pre-shaped lens that 2～20mm does not waits, 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, is graded index self-defocusing glass lens.
Embodiment four
(1) the quartz glass bushing pipe of diameter 45mm, thick 4mm, it is arranged on PCVD equipment, be passed through SiCl4、GeCl4、O2Gas Body, body of heater heating-up temperature 1200 DEG C, under high-frequency microwave effect, start deposition, generate Ge doping SiO2, improve refractive index.Initially GeCl4Content gradually rises to certain value, after be gradually lowered, meanwhile gradually add C2F6+CF4+BCl3, deposit 8 hours, Complete whole deposition process.
(2) after deposition completes, transfer bushing pipe to collapsing stove, collapsing at 2000 DEG C, bushing pipe rotates with 60r/min speed, Design temperature program, after centre initially forms sealing, to both sides extension, of completely closed to central duct, collapsing becomes diameter The GRIN rod of 30mm.
(3) this GRIN rod directly cutting into the pre-shaped lens that 10～50mm does not waits, end face is polished to minute surface, is gradient Refractive index self-defocusing glass lens.Parabolic type region, center is qualified graded index region, and peripheral part is permissible Cut away, it is also possible to as lens packages region, play fixing effect.
It is apparent that the present invention uses PCVD method to manufacture graded index glass lens, can freely be accurately controlled Index distribution, refractive index is centrosymmetric distribution, and different size lens are in preferably cylindric, and above example is only done briefly Explanation.
As it will be easily appreciated by one skilled in the art that and the foregoing is only presently preferred embodiments of the present invention, not in order to Limit the present invention, all any modification, equivalent and improvement etc. made within the spirit and principles in the present invention, all should comprise Within protection scope of the present invention.

Claims (10)

1. the preparation method of graded index quartz glass lens, it is characterised in that using plasma chemical gaseous phase is sunk Amass the quartz glass layer in the doping of glass bushing pipe inside deposition, then collapsing becomes solid gradient index rod in collapsing stove, and directly Connect section or be drawn into section after thin gradient index rod, being finally polished to lens.
2. the preparation method of graded index quartz glass lens according to claim 1, it is characterised in that described bushing pipe Material is quartz, and external diameter is 20～100mm, and thickness is 2～20mm.
3. the preparation method of graded index quartz glass lens according to claim 1 and 2, it is characterised in that wait from The raw material of sub-body chemical vapor phase growing is SiCl4、GeCl4、PCl3、PF3、POCl3、BCl3、BF3、C2F6、CF2Cl2、CF4、SF6、O2 And several combination in He.
4. the preparation method of graded index quartz glass lens according to claim 1 and 2, it is characterised in that wait from The microwave frequency of sub-body chemical vapor phase growing is 2.45GHz, and depositing temperature is 900～1500 DEG C.
5. the preparation method of graded index quartz glass lens according to claim 1 and 2, it is characterised in that sinking During long-pending GRIN Lens, in initial feed, P, B, F constituent content is high, is then gradually lowered, and Ge constituent content gradually rises；Sinking During long-pending self-defocusing lens, in initial feed, Ge constituent content is high, is then gradually lowered, and P, B, F constituent content gradually rises.
6. the preparation method of graded index quartz glass lens according to claim 1 and 2, it is characterised in that deposition Quartz glass layer totally 1000～100000 layers, layer thickness scope is 10nm～10 μm.
7. the preparation method of graded index quartz glass lens according to claim 1 and 2, it is characterised in that collapsing Temperature 1500～2500 DEG C, barred body axial-rotation frequency 10～100r/min, a diameter of 10～50mm after collapsing.
8. the preparation method of graded index quartz glass lens according to claim 1 and 2, it is characterised in that described In collapsing stove, collapsing becomes solid gradient index rod, and gradient index rod vertically draws and attenuates continuously, the graded index after drawing-down Rod diameter range is 0.1～10mm.
9. the preparation method of graded index quartz glass lens according to claim 8, it is characterised in that at collapsing stove During middle collapsing, thermoplastic temperature range is 1600～2200 DEG C, gradient index rod annealing region after drawing-down It is 800～1200 DEG C.
10. the preparation method of graded index quartz glass lens according to claim 1 and 2, it is characterised in that polishing After the surface roughness Ra < 5nm of graded index quartz glass lens.
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