A kind of manufacture method of preform and producing apparatus thereof
Technical field
The manufacture method of a kind of preform of the present invention and producing apparatus thereof relate to preform and make the field, specifically, are to utilize Infrared Thermography Technology to gather powder caput surface temperature, and participate in a kind of method and apparatus of control gas flow.Use this method can accomplish real-time adjustment to gas flow, in order to realize the accurate control to powder rod density, prevent because density gradient causes the powder rod to ftracture greatly, thus the lifting quality product.
Background technology
At present, the gas that the axial vapor deposition method is used, its flow mainly are to control by mass flow controller (being called for short MFC).MFC control flow is by preestablishing several stages, gives constant flow to each stage, and in the deposition process of powder rod, gas is supplied according to preset flow rate.Carry out the control of gas flow by MFC, have a drawback: can not adjust gas flow in real time, be unfavorable for the accurate control to powder rod density.
Have data to show, use the powder rod of axial vapor deposition method preparation, owing to each layer torch flame temperature difference when depositing, its density presents Gradient distribution.As Fig. 1, wherein, 1., 2. two places are intersections of flame.A host of facts show that this two places density is more low, and the probability that cracking takes place is more big.
Chinese invention patent 200610129070.2 has been introduced a kind of by the temperature distribution on the temperature measurement unit detection prefabricated rods vertical axis, and by adjusting gas flow, flame focal length and blowtorch angle, with the method for temperature control in claimed range.But there are two drawbacks in this method.One, what this method caught is temperature on the line, can not reflect the temperature distribution state of whole caput, insensitive to the response of caput variation of temperature.Its two, mention in this method the blowtorch angle adjusted that the adjustment of blowtorch angle can make prefabricated rods caput shape, size generation noticeable change, thereby cause the sandwich layer diameter of prefabricated rods and the ratio of cladding diameter to change.In fact, in scale operation, require the ratio of sandwich layer diameter and cladding diameter should be relatively stable.
Chinese invention patent 200610142065.5 has been introduced a kind of by temperature measurement unit detection prefabricated rods terminal temperature and fibre core temperature of lower, and calculates its difference, controls the method for prefabricated rods axial motion accordingly.But two drawbacks of the same existence of this method.One, what this method caught is temperature on the line, can not reflect the temperature distribution state of whole caput, insensitive to the response of caput variation of temperature.Its two, the real-time speed change in the prefabricated rods production process may cause the considerable change of sandwich layer specific refractory power, makes the axial parameter resistance to overturning of prefabricated rods variation.
Summary of the invention
The present invention seeks at above-mentioned weak point, propose a kind of manufacture method and producing apparatus thereof of preform.The present invention can overcome the problem that current technology can not be adjusted in real time gas flow, powder rod density is accurately controlled, propose a kind of based on the surface temperature acquisition technique, adjust in real time gas flow, accurately control method and the producing apparatus thereof of powder rod density, can prevent effectively that density gradient from causing powder rod cracking greatly, thereby promote quality product.
A kind of manufacture method of preform and producing apparatus thereof are to take following technical scheme to realize:
A kind of producing apparatus of preform comprises tower body, prefabricated rods deposition chamber, motor one, motor two, chuck, screw mandrel, metal suspension rod, guide rail, quartzy cavity, quartzy target rod, quartzy blowtorch one, quartzy blowtorch two, SiCl
4Head tank, GeCl
4Head tank, liquid Ar storage tank, liquid O
2Storage tank, H
2Storage tank, gas housing, magnetic valve one, magnetic valve two, central processing unit, thermal infrared imager, exhaust duct, pre-treatment tower, electric precipitation tower and washing tower.
The prefabricated rods deposition chamber is installed above quartzy cavity, and at the tower body upper mounting rail, chuck links to each other with screw mandrel, and motor one control screw mandrel rotation is so that chuck rises and decline motor two control card disc spins along guide rail.Metal suspension rod clamping is on chuck, and quartzy target rod is packed in the metal suspension rod, is used at the deposition process attaching powder.
Quartzy blowtorch one, quartzy blowtorch two are installed in quartzy cavity right side respectively, and the blowtorch mouth of quartzy blowtorch one and quartzy blowtorch two is in quartzy inside cavity.
SiCl
4Head tank, GeCl
4Head tank, liquid Ar storage tank, liquid O
2Storage tank, H
2Gas in the storage tank enters gas housing inside by pipeline respectively, by mass flow controller MFC control gas flow, and continues to enter quartzy blowtorch one, quartzy blowtorch two through pipeline respectively.
Quartzy cavity left side is equipped with thermal infrared imager, and thermal infrared imager links to each other with central processing unit by signal wire.The H that links to each other with quartzy blowtorch one, quartzy blowtorch two
2Magnetic valve one, magnetic valve two are housed respectively on the pipeline, link to each other with central processing unit by control line.
Described central controller receives the feedback signal of thermal infrared imager, the accounting temperature deviation, and use PlD control principle control H
2Magnetic valve one on the pipeline, magnetic valve two apertures enter the H of quartzy blowtorch one, quartzy blowtorch two with adjusting
2Airshed.Described central controller adopts the CP350/370 family computer of being made by CHINO company, and PID controller (proportional-integral derivative controller) is installed, and is provided with sequence of control.
Quartzy cavity upper left quarter is provided with exhaust duct, and exhaust duct is connected with the pre-treatment tower, and the pre-treatment tower links to each other with the electric precipitation tower by pipeline, and the electric precipitation tower links to each other with washing tower by pipeline, for the tail gas of collecting, the processing reaction process produces.
Some mass flow controller MFC are installed, by its flow of time variable control that is installed on the master control cabinet computer in the described gas housing.
A kind of manufacture method of preform is as follows:
1. gas supply
With SiCl
4Head tank, GeCl
4Head tank, liquid Ar storage tank, liquid O
2Storage tank, H
2Gas in the storage tank enters gas housing inside by pipeline respectively, by mass flow controller MFC control gas flow, and continues to enter quartzy blowtorch one, quartzy blowtorch two through pipeline.Wherein, the mass flow controller MFC(that each gas pipeline (gas circuit) upward disposes is AE FC-7800CD series mass flow director for example), for the airshed of control different steps.
SiCl
4Flow can be adjusted between 0.1g/min~20g/min, and flame hydrolysis generates SiO under high-temperature condition
2, be used to form covering and the sandwich layer of prefabricated rods; GeCl
4Flow can be adjusted between 0.01g/min~1.0g/min, and flame hydrolysis generates GeO under high-temperature condition
2, be entrained in sandwich layer to improve the sandwich layer specific refractory power.Carry SiCl
4, GeCl
4Pipe surface need lay the heating zone, temperature is controlled at 100 ℃
H
2Flow can be adjusted between 0.1L/min~30L/min; O
2Flow can be adjusted between 0.1L/min~50L/min, wherein, and H
2Play the burning effect, O
2Play combustion-supporting effect, in addition, in order to allow H
2Complete reaction, when flow set, need be with O
2It is more than needed that flow set becomes.
The Ar flow can be adjusted between 10L/min at 0.1L/min.Effect has two: one, as carrier gas, and delivery unstripped gas; Two, with H
2, O
2Separate, prevent that it from mixing, reacting in blowtorch.
2. deposited powder rod
The metal suspension rod of at first a quartzy target rod that be used for to pile up powder being packed into is opened motor one, make the metal suspension rod drop to specified location after, open motor two, make the rotation of metal suspension rod.Igniting soon begins flame hydrolysis, and powder begins to be deposited on quartzy target rod surface.Open automatic control mode cashier's office in a shop in master control, after the operation sequence of control, the metal suspension rod draws the rotation of quartzy target rod and rises, and wherein sequence of control is formed by Visual Basic software editing, is connected with equipment by signal wire.
In deposition process, need be with pressure-controlled in the quartzy cavity a metastable scope, the metal suspension rod keeps certain speed of rotation and pulling speed.Wherein, pressure-controlled is at 30 ± 5Pa in the quartzy cavity, and speed of rotation is controlled at 10rpm, and pulling speed is controlled at 35mm/h.
3. the collection of thermal-induced imagery and feedback control
Pass through thermal infrared imager, gather powder caput surface temperature, carry out the A/D conversion, and by data line with the digital data transmission that converts to central processing unit, changed by central processing unit analysed for powder caput surface temperature, and send action command, the valve opening of control magnetic valve, magnetic valve, thereby reach the purpose of real-time adjustment gas flow, make preform.
4. exhaust collection, processing
By vapor pipe, tail gas is transported to waste gas treatment equipment handles.Waste gas treatment equipment comprises pre-treatment tower, electric precipitation tower and washing tower.Wherein, the pre-treatment tower mainly acts on and is, to the tail gas processing of lowering the temperature; The electric precipitation tower mainly acts on, and by electrion, makes dust charged and with its absorption; Washing tower mainly acts on, and utilizes the sour gas such as HCl, HF in NaOH solution and the tail gas to carry out neutralization reaction.By above a series for the treatment of measures, make tail gas reach emission standard.
Manufacture method and the producing apparatus thereof of preform of the present invention are reasonable in design, the present invention can overcome the problem that current technology can not be adjusted in real time gas flow, powder rod density is accurately controlled, propose a kind of based on the surface temperature acquisition technique, adjust in real time gas flow, accurately control method and the producing apparatus thereof of powder rod density, can prevent effectively that density gradient from causing powder rod cracking greatly, thereby promote quality product.
The manufacture method of preform of the present invention and producing apparatus advantage thereof are:
1. in whole deposition process, utilize the surface temperature acquisition technique of infrared thermal imagery, can obtain powder caput surface temperature change in real time, and in time respond, adjust gas flow, thereby powder caput temperature control in a metastable scope, is prevented the noticeable change of the density brought greatly owing to range of temperature, make the density of the powder rod Adjustable real-time and controlled that becomes;
2. by this method, can accurately control the density of powder rod, avoid density gradient between layer and the layer
3. cause powder rod cracking greatly, thereby promote quality product.Simultaneously, allow whole prefabricated rods manufacturing processed become automatization more, intellectuality.
Description of drawings
Fig. 1 is powder rod density distribution synoptic diagram, and wherein transverse axis is represented the lateral radius of powder rod, and the longitudinal axis is represented the density on the powder rod cross section.
1., what 2. mark is respectively the intersection of several blowtorch among Fig. 1,, cracking occurs in herein easily.
Fig. 2 is equipment synoptic diagram of the present invention.
Fig. 3 is the loop control theory figure that the present invention relates to.
Fig. 4 is PID control principle figure, and wherein, R (t) is set-point, and Y (t) is the real output value of system.Deviate E (t)=Y (t)-R (t), deviate E (t) are as the input of PID controller, and U (t) is as the output of PID controller and the input of controlled plant.Among the present invention, ratio P, integration I, differential D can regulate in 0.1%~100%, 0.01~60,0.01~10 scope respectively.
Fig. 5 is the powder rod density profile of embodiment one.
Fig. 6 is the powder rod density profile of embodiment two.
Embodiment
With reference to accompanying drawing 1~6, a kind of producing apparatus of preform comprises tower body 1, prefabricated rods deposition chamber 2, motor 1, motor 24, chuck 5, screw mandrel 6, metal suspension rod 7, guide rail 8, quartzy cavity 9, quartzy target rod 10, quartzy blowtorch 1, quartzy blowtorch 2 12, SiCl
4 Head tank 13, GeCl
4 Head tank 14, liquid Ar storage tank 15, liquid O
2Storage tank 16, H
2Storage tank 17, gas housing 18, magnetic valve 1, magnetic valve 2 20, central processing unit 21, thermal infrared imager 22, exhaust duct 23, pre-treatment tower 24, electric precipitation tower 25 and washing tower 26.
Prefabricated rods deposition chamber 2 is installed above quartzy cavity 9, and at tower body 1 upper mounting rail 8, chuck 5 links to each other with screw mandrel 6, and 6 rotations of motor one 3 control screw mandrels are so that chuck 5 rises and descends along guide rail 8,5 rotations of motor 24 control chucks.Metal suspension rod 7 clampings are on chuck 5, and quartzy target rod 10 is packed in the metal suspension rod 7, are used at the deposition process attaching powder.
Quartzy blowtorch 11, quartzy blowtorch 12 are installed in quartzy cavity 9 right sides respectively, and the blowtorch mouth is in quartzy cavity 9 inside.SiCl
4 Head tank 13, GeCl
4 Head tank 14, liquid Ar storage tank 15, liquid O
2Storage tank 16, H
2Gas in the storage tank 17 enters gas housing 18 inside by pipeline respectively, by mass flow controller MFC28~36 control gas flows, and continues to enter quartzy blowtorch 1, quartzy blowtorch 2 12 through pipeline respectively.
Quartzy cavity 9 left sides are equipped with thermal infrared imager 22, and thermal infrared imager 22 links to each other with central processing unit 21 by signal wire.The H that links to each other with quartzy blowtorch 1, quartzy blowtorch 2 12
2 Magnetic valve 1, magnetic valve 2 20 are housed respectively on the pipeline, link to each other with central processing unit 21 by control line.
Described central controller 21 receives the feedback signal of thermal infrared imager 22, the accounting temperature deviation, and use PlD control principle control H
2 Magnetic valve 1 on the pipeline, magnetic valve 2 20 apertures enter the H of quartzy blowtorch 1, quartzy blowtorch 2 12 with adjusting
2Airshed.Described central controller adopts the CP350/370 family computer of being made by CHINO company, and PID controller (proportional-integral derivative controller) is installed, and is provided with sequence of control.
Quartzy cavity 9 upper left quarters are provided with exhaust duct 23, exhaust duct 23 is connected with pre-treatment tower 24, pre-treatment tower 24 links to each other with electric precipitation tower 25 by pipeline, and electric precipitation tower 25 links to each other with washing tower 26 by pipeline, for the tail gas of collecting, the processing reaction process produces.
In the described gas housing 18 mass flow controller MFC28, MFC29, MFC30, MFC31, MFC32, MFC33, MFC34, MFC35, MFC36 are installed, by the flow of master control cabinet 37 these 9 MFC of control.
A kind of manufacture method of preform is as follows:
1, gas supply
As Fig. 2, with SiCl
4 Head tank 13, GeCl
4 Head tank 14, liquid Ar storage tank 15, liquid O
2Storage tank 16, H
2Gas in the storage tank 17 enters gas housing 18 inside by pipeline respectively, by mass flow controller MFC28~36 control gas flows, and continues to enter quartzy blowtorch 1, quartzy blowtorch 2 12 through pipeline.Wherein, the mass flow controller MFC(that each gas pipeline (gas circuit) upward disposes is AE FC-7800CD series mass flow director for example), for the airshed of control different steps.
SiCl
4Flow can be adjusted between 0.1g/min~20g/min), flame hydrolysis generates SiO under high-temperature condition
2, be used to form covering and the sandwich layer of prefabricated rods; GeCl
4Flow can be adjusted between 0.01g/min~1.0g/min, and flame hydrolysis generates GeO under high-temperature condition
2, be entrained in sandwich layer to improve the sandwich layer specific refractory power.Carry SiCl
4, GeCl
4Pipe surface need lay the heating zone, temperature is controlled at 100 ℃
H
2Flow can be adjusted between 0.1L/min~30L/min; O
2Flow can be adjusted between 0.1L/min~50L/min, wherein, and H
2Play the burning effect, O
2Play combustion-supporting effect, in addition, in order to allow H
2Complete reaction, when flow set, need be with O
2It is more than needed that flow set becomes.
The Ar flow can be adjusted between 10L/min at 0.1L/min.Effect has two: one, as carrier gas, and delivery unstripped gas; Two, with H
2, O
2Separate, prevent that it from mixing, reacting in blowtorch.
2, deposited powder rod
The metal suspension rod 7 of at first a quartzy target rod 10 that be used for to pile up powder being packed into is opened motor 1, make metal suspension rod 7 drop to specified location after, open motor 24, make 7 rotations of metal suspension rod.Igniting soon begins flame hydrolysis, and powder begins to be deposited on quartzy target rod 10 surfaces.Open automatic control mode at master control cabinet 36, after the operation sequence of control, quartzy target rod 10 rotations of metal suspension rod 7 tractions and rising, wherein, sequence of control is formed by Visual Basic software editing, is connected with equipment by signal wire.
In deposition process, need be with pressure-controlled in the quartzy cavity 9 a metastable scope, metal suspension rod 7 keeps certain speed of rotation and pulling speed.Wherein, pressure-controlled is at 30 ± 5Pa in the quartzy cavity 9, and speed of rotation is controlled at 10rpm, and pulling speed is controlled at 35mm/h.
3, the collection of thermal-induced imagery and feedback control
By thermal infrared imager 22, gather powder caput surface temperature, carry out the A/D conversion, and by data line with the digital data transmission that converts to central processing unit 21, changed by central processing unit 21 analysed for powder caput surface temperatures, and send action command, the valve opening of control magnetic valve 1, magnetic valve 2 20, thereby reach the purpose of real-time adjustment gas flow, make preform.
4, exhaust collection, processing
By vapor pipe 23, tail gas is transported to waste gas treatment equipment handles.Waste gas treatment equipment comprises pre-treatment tower 24, electric precipitation tower 25, washing tower 26.Wherein, the main effect of pre-treatment tower 24 is, to the tail gas processing of lowering the temperature; The main effect of electric precipitation tower 25 is, by electrion, makes dust charged and with its absorption; Washing tower 26 main effects are to utilize the sour gas such as HCl, HF in NaOH solution and the tail gas to carry out neutralization reaction.By above a series for the treatment of measures, make tail gas reach emission standard; Described pre-treatment tower 24, electric precipitation tower 25 and washing tower 26 adopt commercially available coordinative composition of equipments to use.
The raw material that the present invention relates to comprises: one, SiCl
4(flow can be adjusted between 0.1g/min~20.0g/min), flame hydrolysis generates SiO under high-temperature condition
2, be used to form covering and the sandwich layer of prefabricated rods; Two, GeCl
4(flow can be adjusted between 0.01g/min~1.00g/min), flame hydrolysis generates GeO under high-temperature condition
2, be entrained in sandwich layer to improve the sandwich layer specific refractory power.
Fuel comprises: H
2(flow can be adjusted between 0.1L/min~30.0L/min), O
2(flow can be adjusted between 0.1L/min~50.0L/min), wherein, H
2Play the burning effect, O
2Play combustion-supporting effect.In addition, in order to allow H
2Complete reaction, when flow set, need be with O
2It is more than needed that flow set becomes.
Auxiliary material comprises: the Ar(flow can be adjusted between 10.0L/min at 0.1L/min).Effect has two: one, as carrier gas, and delivery unstripped gas; Two, with H
2, O
2Separate, prevent that it from mixing, reacting in blowtorch.
Raw material, fuel and auxiliary material are delivered to the blowtorch mouth and react through piping, constantly are stacked on the target rod, are shaped to the powder rod, and continue growth.Wherein, the pipeline of transferring raw material needs the external application heating zone, and temperature is controlled at 100 ℃.
Embodiment one:
At the quartzy target rod 10 of a long 500mm of metal suspension rod 7 installations, be the SiCl of 0.1g/min with initial flow
4, 0.01g/min GeCl
4, the Ar of 1.0L/min, the O of 5.0L/min
2H with 3.0L/min
2Feed quartzy blowtorch 2 12, generate SiO by flame hydrolysis
2, GeO
2, be attached to quartzy target rod 10 lower ends, form sandwich layer.Feed the SiCl of initial flow 0.1g/min in the quartzy blowtorch 11
4, the Ar of 1.0L/min, the O of 15.0L/min
2H with 10.0L/min
2, generate SiO by flame hydrolysis
2, the covering of formation prefabricated rods.Each stage flow set such as following table 1:
Table 1
As Fig. 2, by 7 rotations of chuck 5 control metal suspension rods, metal suspension rod 7 is drawing quartzy target rod 10 and is rising along guide rail 8, and wherein speed of rotation control is at 10rpm, and pulling speed is controlled at 35mm/h.Pressure-controlled is at 30 ± 5Pa in the quartzy cavity 9.
At H
2On the pipeline, magnetic valve 1, magnetic valve 2 20 are installed, valve opening is subjected to central processing unit 21 controls.Wherein, parameter P is set at 10%, and parameter I is set at 60, and parameter D is set at 3.Magnetic valve 1, magnetic valve 2 20, central processing unit 21, thermal infrared imager 22, powder rod 27 constitute a closed loop control system.As Fig. 3, by thermal infrared imager 22 powder that collects rod 27 caput surface temperatures are fed back to central processing unit 21, calculate deviate, wherein, the medial temperature in the infrared thermal imagery picture is set at 1050 ℃, and deviation standard is decided to be ± and 10 ℃.When medial temperature was lower than 1040 ℃, the output bias signal sent instruction by the PID controller, increased magnetic valve 1, magnetic valve 2 20 valve openings to increase H
2Flow, thus temperature improved, and in like manner, when medial temperature was higher than 1060 ℃, the output bias signal sent instruction by the PID controller, reduced magnetic valve 1, magnetic valve 2 20 valve openings to reduce H
2Flow, thus temperature reduced.When temperature was between 1040~1060 ℃, magnetic valve 1, magnetic valve 2 20 valve openings remained unchanged.Wherein, data acquiring frequency is set at 1 time/min.
Accompanying drawing 4 is each layer density of the powder rod that makes according to the method described above.The result shows: the blowtorch intersection 1., 2. density reaches 0.24g/cm3,0.27g/cm3 respectively.The intersection width is 1.5mm, 1.5mm.
Embodiment two:
At the quartzy target rod 10 of a long 500mm of metal suspension rod 7 installations, be the SiCl of 0.1g/min with initial flow
4, 0.01g/min GeCl
4, the Ar of 1.0L/min, the O of 6.0L/min
2H with 4.0L/min
2Feed quartzy blowtorch 2 12, generate SiO by flame hydrolysis
2, GeO
2, be attached to quartzy target rod 10 lower ends, form sandwich layer.Feed the SiCl of initial flow 0.1g/min in the quartzy blowtorch 1
4, the Ar of 1.0L/min, the O of 20.0L/min
2H with 15.0L/min
2, generate SiO by flame hydrolysis
2, the covering of formation prefabricated rods.Each stage flow set such as following table 2:
Table 2
As Fig. 2, by 7 rotations of chuck 5 control metal suspension rods, metal suspension rod 7 is drawing quartzy target rod 10 and is rising along guide rail 8, and wherein speed of rotation control is at 10rpm, and pulling speed is controlled at 35mm/h.Pressure-controlled is at 30 ± 5Pa in the quartzy cavity 9.
At H
2On the pipeline, magnetic valve 1, magnetic valve 2 20 are installed, valve opening is subjected to central processing unit 21 controls.Wherein, parameter P is set at 10%, and parameter I is set at 30, and parameter D is set at 3.Magnetic valve 1, magnetic valve 2 20, central processing unit 21, thermal infrared imager 22, powder rod 27 constitute a closed loop control system.As Fig. 3, by thermal infrared imager 22 powder that collects rod 27 caput surface temperatures are fed back to central processing unit 21, calculate deviate, wherein, the medial temperature in the infrared thermal imagery picture is set at 1080 ℃, and deviation standard is decided to be ± and 5 ℃.When medial temperature was lower than 1075 ℃, the output bias signal sent instruction by the PID controller, increased magnetic valve 1, magnetic valve 2 20 valve openings to increase H
2Flow, thus temperature improved, and in like manner, when medial temperature was higher than 1085 ℃, the output bias signal sent instruction by the PID controller, reduced magnetic valve 1, magnetic valve 2 20 valve openings to reduce H
2Flow, thus temperature reduced.When temperature was between 1075~1085 ℃, magnetic valve 1, magnetic valve 2 20 valve openings remained unchanged.Wherein, data acquiring frequency is set at 2 times/min.
What accompanying drawing 5 showed is each layer of powder rod density of example two correspondences, and the result shows: the blowtorch intersection 1., 2. density reaches 0.30g/cm3,0.34g/cm3 respectively.The intersection width is 0.5mm, 0.5mm.
Through comparing with example one, as can be seen, embodiment two is by increasing H
2, O
2Flow increases average design temperature, revises deviate, and improves a series of measures of data acquiring frequency, and is final: the density that one, has improved each layer of powder rod; Two, the blowtorch intersection 1., obviously change is big for powder density 2., and the density difference with Core and Clad dwindles simultaneously, and thickness reduces to some extent.