CN1123648C - Improved chemical vapor-phase deposition method by uisng graphite heating furnace as hot source - Google Patents
Improved chemical vapor-phase deposition method by uisng graphite heating furnace as hot source Download PDFInfo
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- CN1123648C CN1123648C CN 01133608 CN01133608A CN1123648C CN 1123648 C CN1123648 C CN 1123648C CN 01133608 CN01133608 CN 01133608 CN 01133608 A CN01133608 A CN 01133608A CN 1123648 C CN1123648 C CN 1123648C
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- chemical vapor
- present
- deposition
- deposition method
- optical fiber
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- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 39
- 239000010439 graphite Substances 0.000 title claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000010438 heat treatment Methods 0.000 title description 10
- 239000000126 substance Substances 0.000 title 1
- 238000001947 vapour-phase growth Methods 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 44
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 238000000151 deposition Methods 0.000 claims abstract description 26
- 230000008021 deposition Effects 0.000 claims abstract description 24
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims description 16
- 230000006698 induction Effects 0.000 claims description 2
- 239000013307 optical fiber Substances 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 29
- 239000010453 quartz Substances 0.000 description 23
- 238000005137 deposition process Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 239000000835 fiber Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 238000007906 compression Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- 240000008042 Zea mays Species 0.000 description 2
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 235000009973 maize Nutrition 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 125000003003 spiro group Chemical group 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 210000005069 ears Anatomy 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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Abstract
The present invention discloses an improved chemical vapor deposition method using a graphite heater furnace as a heat source. The present invention is characterized in that a graphite heater furnace is used as a heat source, and an improved chemical vapor deposition method is adopted to manufacture an optical fiber preform. The present invention comprises the following steps: a. deposition reaction occurs in the raw materials which react, so that a deposition liner tube is produced; B. the deposition liner tube is melted and shrunk into a solid core rod. The present invention solves the problems in the existing methods that oxyhydrogen flame is used as a heat source, a big safe hidden danger exists, and the optical fiber performance is affected, which are caused because hydrogen is used for a long time. The present invention improves the performance of the optical fiber preform, also improves the performance of the optical fiber, increases the deposition rate, saves equipment investment expense and running expense, and has great economic benefits.
Description
Technical field
The present invention relates to the manufacture method of preform, especially is the method for the modified chemical vapor deposition manufacturing preform of thermal source with the graphite heater furnace.
Background technology
Be used for manufacturers at present and be mainly chemical vapor deposition method with the processing method of fossil English optical fiber, this method is divided into method and the outer method of pipe in the pipe.For managing outer method, its main technique method has outer vapour deposition process of pipe and axle two kinds of vapour deposition processes mutually, mainly comprises two kinds of plasma chemical vapor deposition and modified chemical vapor deposition process (MCVD)s and manage interior method.The modified chemical vapor deposition method be the MCVD method be 1974 by U.S. AT﹠amp; The classical technology of the people such as Machesney of T company Bell Laboratory exploitation is to be used to one of processing method of making silica fibre in the world the earliest, and up to this point, it is one of topmost methods for optical fiber manufacture in the world still.Optical fiber with this method manufacturing accounts for about 25% of whole silica fibre output.Common MCVD method be a kind of be thermal source with the oxyhydrogen flame, occur in the gas deposition that carries out in the high-purity quartz glass pipe.The chemical reaction mechanism of MCVD method is a high temperature oxidation.MCVD technology is by depositing and becoming two processing steps of rod to form.Deposition process is
In order to obtain the fiber cores index distribution of design requirements, becoming rod motion is the molten plug that shortens a solid preform into of hollow purity quartz glass pipe for high that will deposit.
The thermal source that the MCVD method adopts is based on oxyhydrogen flame; To oxyhydrogen flame is main thermal source, has certain defective, mainly shows as:
When the first, reaching certain limit, can blast, make for a long time because of the aerial concentration of hydrogen
Then there is huge potential safety hazard with hydrogen;
The second, can produce a large amount of heats and waste gas during combustion of hydrogen, for keeping the temperature of operating environment
With humidity, need these waste gas exhausts are handled, can increase the corresponding apparatus investment like this
With working cost.
Three, the preform that uses oxyhydrogen flame to produce as thermal source, because of its outside surface long-time
Be in pyritous steam and the hydrogen environment, so in manufacturing processed, hydrogen atom can be not
Disconnected inwardly spreads, and the feasible optical fiber of being made by this prefabricated rods is because of OH exists
The 1385nm place has higher absorption peak, so near the decay meeting of optical fiber 1385nm
Significantly increase.Can influence near the window of transmission system 1385nm like this, and
Transmission performance generation to other service bands (as 1310nm to 1550nm) is unfavorable
Influence.
Summary of the invention
Goal of the invention of the present invention is exactly the defective at aforesaid method, has proposed a kind ofly to make preform with graphite heater furnace as the modified chemical vapor deposition of thermal source, to remedy the deficiency of aforesaid method.
Adopt two-step approach when the inventive method is made preform: the first step is deposition, produces the deposition bushing pipe by the raw material generation deposition reaction of reaction; Second goes on foot to becoming rod, the deposition bushing pipe is melted shorten solid plug into.Particularly be: with the raw material such as the SiCl of reaction
4, O
2Also has a spot of hotchpotch GeCl
4, fluorine Lyons, Cl
2Highly purifiedly ceaselessly rotating in the quartz liner Deng introducing one around axial; As reaction, sintering is ceaselessly moving along quartz liner lentamente to and fro with thermal source-graphite heater furnace in becoming rod motion, when reaction mass flows to the heating region of graphite heater furnace, in the time of about 1600 ℃, reaction mass just reacts and generates pulverous reactant, with air-flow drift backward, and lower, be positioned on the tube wall of lower edge of conversion zone to get off with Powdered deposition in temperature.When graphite heater furnace moved to this zone, under action of high temperature, this powder was sintered into transparent glass.Like this, along with graphite heater furnace ceaselessly moves lentamente to and fro along quartz liner, will ceaselessly deposit according to designing institute requirement ground reactant at the bushing pipe inwall.After deposition process is finished, will become the desired gas of rod motion, as Cl
2Deng introducing in this quartz liner, and stop to import reactor feed gas in the deposition process simultaneously; Regulate the temperature of graphite heater furnace, the temperature height the when temperature of graphite heater furnace is normally than deposition reaction at this moment.Under action of high temperature, shorten solid ear of maize into this quartz liner is molten; By the temperature of control graphite heater furnace and the pressure in the quartz liner, the molten speed that contracts of may command quartz liner.In order to control the deformation of quartz liner in molten compression process, and then after being controlled to rod, the circularity of the sandwich layer of plug; Quartz liner needs to shrink lentamente step by step, promptly along with graphite heater furnace constantly moves lentamente to and fro along quartz liner, reacts the most at last that bushing pipe is molten to shorten solid plug into.
Adopting MCVD device of the present invention to produce preform has the following advantages: the first, removed when using oxyhydrogen flame as thermal source the huge potential safety hazard that exists because of life-time service hydrogen; The second, reduced because of using oxyhydrogen flame to be thermal source, needed pump drainage to handle the waste gas that the oxyhydrogen flame burning produces, and required facility investment and working cost.Three, improved the performance of preform; When adopting the preform of the present invention's production,
Because of in deposition process and molten compression process, the bushing pipe of reaction is heated evenly, heating surface area
Greatly, so on technology, be easy to guarantee the radial symmetry and the prefabricated rods of preform
Axial homogeneity; Four, improved optical fiber properties; Its surperficial hydrogen of preform that adopts the present invention to produce
The content of oxygen root OH can by to adopt oxyhydrogen flame be the preform produced of thermal source up to
Approximately be reduced to below the 1ppm about 1000ppm.The optical fiber that adopts the present invention to produce
The decay meeting of prefabricated rods and the optical fiber that is drawn into is by tangible reduction.In addition, predispersed fiber
The radial symmetry of system rod has significant effects, predispersed fiber to the polarization mode dispersion of optical fiber
It is the prerequisite that obtains good polarization mode dispersion that the system rod has good radial symmetry.
Preform have good axial homogeneity can guarantee optical fiber have good all
Even performance.Five, improved sedimentation rate; When adopting the preform of the present invention's production, because of depositing
In the process, the bushing pipe of reaction is heated evenly, and heating surface area is big, and normally oxyhydrogen flame is
More than the twice of thermal source, thus can make reaction zone strengthen, and reaction zone temperature distributes all
Even; On the other hand, because the heating zone is big, so can make thermal source move on to behind the reaction zone
During sedimentary province, can sinter the powdered reactant in the sedimentary province into glass at faster speed
The glass attitude, thus have when having guaranteed to adopt the preform that the present invention produces higher
Sedimentation rate.So just, can reduce the manufacturing cost of optical fiber, and improve single device
Throughput.
Description of drawings Fig. 1 is the synoptic diagram of level deposition reaction equipment therefor of the present invention.Fig. 2 is the synoptic diagram of vertical deposition reaction equipment therefor of the present invention.Fig. 3 is a deposition reaction process synoptic diagram of the present invention.Fig. 4 becomes the synoptic diagram of rod motion for the present invention
Embodiment
Below in conjunction with accompanying drawing, enumerate part embodiment the present invention be described further:
Embodiment one
As shown in Figure 1, horizontal fixed is being set up the quartz liner 102 that is used for deposition reaction on MCVD machine tool 101.Have a heat affected zone 103 in the quartz liner, the heat of heat affected zone is then produced by heating medium 104.Heating installation of the present invention is the graphite resistance process furnace, is heating element with the graphite component, is the tubular oven of lining with graphite component or other.Deposition with become rod motion, quartz liner is the middle body that is positioned at the graphite resistance process furnace; And rotating incessantly, shown in rotation arrow 105a among the figure.As described above, the heat affected zone 103 of quartz liner is that the graphite resistance process furnace then is fixed on the spiro driving device 106 by due to the heating of graphite resistance process furnace.Spiro driving device 106 can be flatly at the uniform velocity mobile to and fro on the MCVD machine tool; Thereby it is axially at the uniform velocity mobile to and fro along bushing pipe to drive the graphite resistance process furnace, shown in arrow 105b.The various piece that is positioned at graphite resistance process furnace zone of action quartz liner so all can be subjected to heating equably.
The inlet end 107 of MCVD machine tool is connected with raw material cabinet 108.Reaction raw materials vapour in the raw material cabinet 108 just inlet end 107 by the MCVD machine tool enters reaction bushing pipe 102.Raw material cabinet 108 comprises the import 109 of one road oxygen; Two- way oxygen intake 110 and 111 links to each other with 115 with head tank 114 respectively in addition, in the direct incoming stock liquid 116 of tubular stinger and 117, bubbling takes place in stock liquid; Like this, when this two-way oxygen, when head tank 114 and 115 comes out, carrying the raw material 116 and 117 of steam state respectively.Raw material from head tank 113 merges together the entrance end that enters the MCVD machine tool by its outlet pipe 112 with above-mentioned two-way gas.
Giving vent to anger of system be exit end 118 by the MCVD machine tool, links to each other with extraneous evacuation system and gone out by pump drainage.
As shown in Figure 2, the present invention also can adopt the vertical deposition reaction unit.From the performance characteristic aspect, this device is similar with device shown in Figure 1.Quartz liner 102 is to be fixed on the MCVD machine tool by chuck 221 and 222, and inlet mouth 226 is to link to each other with raw material cabinet 108, and giving vent to anger is by air outlet 227, links to each other with extraneous evacuation system and is gone out by pump drainage.
Process when technology of the present invention is carried out deposition reaction after 124 energisings of graphite resistance process furnace, will heat the reaction bushing pipe as shown in Figure 3, and its heat sees through the tube wall of bushing pipe and forms hot-zone 332; Reaction raw materials is entered bushing pipe by entrance end, the direction shown in 334 arrows among the figure flows into.When it flows into hot-zone 332, react, form the strong reactant of powder, and with air-flow drift downstream; At this moment, be full of the powder of drift in reaction hot-zone 332 and its downstream area 335, the powder of part is then under deposition on the tube wall.Powder under deposition on the tube wall can be melt into transparent glass 336 under action of high temperature.
After deposition process is finished, will become the desired gas of rod motion, as Cl
2Deng introducing in this quartz liner, and stop to import reactor feed gas in the deposition process simultaneously; Regulate the temperature of graphite resistance process furnace 124, the temperature height the when temperature of graphite resistance process furnace 124 is normally than deposition reaction at this moment.Under action of high temperature, will have the quartz liner 102 molten solid ears of maize 402 that shorten into of certain thickness settled layer 401; By the temperature of control graphite resistance process furnace and the pressure in the quartz liner, the molten speed that contracts of may command quartz liner.In order to control the deformation of quartz liner in molten compression process, and then after being controlled to rod, the circularity of the sandwich layer of plug; Quartz liner needs to shrink lentamente step by step, promptly along with the graphite resistance process furnace constantly moves lentamente to and fro along quartz liner, reacts the most at last that bushing pipe is molten to shorten solid plug into.
Embodiment two
Another embodiment of the present invention is to change the graphite resistance process furnace among the embodiment one into the graphite induction heater, and other operation is identical.
Claims (4)
1, a kind of is the modified chemical vapor deposition method of thermal source with the graphite heater furnace, it is characterized in that: it is to be thermal source with the graphite heater furnace, adopts the modified chemical vapor deposition method to make preform, and it may further comprise the steps:
A produces the deposition bushing pipe by the raw material generation deposition reaction of reaction;
B will deposit that bushing pipe is molten to shorten solid plug into.
2, a kind of of claim 1 is the modified chemical vapor deposition method of thermal source with the graphite heater furnace, it is characterized in that: deposition reaction and molten contract that all to adopt graphite heater furnace be thermal source.
3, claim 1 or 2 a kind of be the modified chemical vapor deposition method of thermal source with the graphite heater furnace, it is characterized in that: graphite heater furnace is the graphite resistance process furnace.
4, claim 1 or 2 a kind of be the modified chemical vapor deposition method of thermal source with the graphite heater furnace, it is characterized in that: graphite heater furnace is the graphite induction heater.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01133608 CN1123648C (en) | 2001-10-29 | 2001-10-29 | Improved chemical vapor-phase deposition method by uisng graphite heating furnace as hot source |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01133608 CN1123648C (en) | 2001-10-29 | 2001-10-29 | Improved chemical vapor-phase deposition method by uisng graphite heating furnace as hot source |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1354277A CN1354277A (en) | 2002-06-19 |
| CN1123648C true CN1123648C (en) | 2003-10-08 |
Family
ID=4671955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01133608 Expired - Lifetime CN1123648C (en) | 2001-10-29 | 2001-10-29 | Improved chemical vapor-phase deposition method by uisng graphite heating furnace as hot source |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1123648C (en) |
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2001
- 2001-10-29 CN CN 01133608 patent/CN1123648C/en not_active Expired - Lifetime
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| Publication number | Publication date |
|---|---|
| CN1354277A (en) | 2002-06-19 |
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| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: YANGTZE OPTICAL FIBRE AND CABLE CO., LTD Free format text: FORMER NAME: CHANGFEI FIBRE-OPTICAL + OPTICAL CABLE CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: Two road 430073 Hubei city of Wuhan Province, No. 4 Patentee after: Yangtze Optical Fibre and Cable Co., Ltd Address before: Two road 430073 Hubei city of Wuhan Province, No. 4 Patentee before: Changfei Fibre-Optical & Optical Cable Co., Ltd. |
|
| CX01 | Expiry of patent term |
Granted publication date: 20031008 |
|
| CX01 | Expiry of patent term |