CN1477416A - Forming method of zirconium oxide ceramic insertion needle for fibre-optic connector and its equipment - Google Patents

Forming method of zirconium oxide ceramic insertion needle for fibre-optic connector and its equipment Download PDF

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Publication number
CN1477416A
CN1477416A CNA031459544A CN03145954A CN1477416A CN 1477416 A CN1477416 A CN 1477416A CN A031459544 A CNA031459544 A CN A031459544A CN 03145954 A CN03145954 A CN 03145954A CN 1477416 A CN1477416 A CN 1477416A
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die
forming method
punch
contact pin
zirconium oxide
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CN1200297C (en
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勇 黄
黄勇
马天
杨金龙
赵雷
王铁超
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Tsinghua University
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Tsinghua University
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Abstract

The present invention relates to a zirconium oxide ceramic insertion needle forming method and its equipment. The zirconium oxide ceramic insertion needle can be used as optical fibre connector and is made up by adopting the following steps: using organic monomer, cross-linking agent and deionized water and making them into premixed material, then adding ceramic powder body, ball-grinding, adding catalyst and initiator, injecting the above-mentioned mixed slurry material into mould cavity, forming to obtain blank body, drying and sintering so as to obtain the invented product.

Description

The joints of optical fibre forming method and the device of zirconium oxide ceramic contact pin
Technical field
The present invention relates to a kind of forming method and device of zirconium oxide ceramic contact pin, especially relate to forming method and the device of the high joints of optical fibre of a kind of dimension precision requirement, belong to the ceramic component preparing technical field with zirconium oxide ceramic contact pin.
Background technology
The high speed development inevitable requirement information of world economy also will be linked up at a high speed, and the information highway that therefore develops high-performance, two-forty has become from now on the competitively strategic objective of research and development of countries in the world.Optical fiber communication is the main body and the skeleton of information transmission network and information highway, and this Progress in technique always is closely connected together with the progress of base light device, and can further promote the development of optical device technology and industry.The joints of optical fibre are widely used in optical communication system, optical information processing system, optical instrument instrument, it is commonly used to realize from the light source to optical fiber, from the optically-coupled between fiber-to-fiber and optical fiber and the detector, particularly in optical communication system, the optical passive component of the joints of optical fibre amount of being to use maximum.
The contact pin that two optical fiber are achieved a butt joint is the critical component of the joints of optical fibre, and two optical fiber precision by two contact pins 1 is to fetching the continuous transmission (Fig. 1) that realizes signal in the optical fiber 2.Contact pin should have high dimensional accuracy (Fig. 2) and usability stability, therefore material has been proposed very harsh requirement.The contact pin material is mainly contained following requirement: (1) optical fiber wants to pass at an easy rate the micropore of contact pin body.(2) the contact pin body material machining precision that should be able to obtain high machining accuracy, particularly endoporus and right alignment should guarantee in 1 μ m.(3) contact pin body material should have enough intensity and wearing quality, does not lose efficacy in installation, dismounting and use; When being subjected to accidental shock, do not rupture.(4) contact pin body material should have the linear expansion coefficient close with optical fiber, and when environment temperature changed, the contraction of contact pin and expansion and optical fiber were basic identical, to guarantee the tight contact of fiber end face, prevents the loss of light signal.
Partially stabilized zirconia (PSZ) contact pin accounts for more than 95% of whole contact pin market at present.PSZ becomes the main flow material of making contact pin, and mainly contain following reason: 1) zirconia ceramics is easy to obtain crystallite, and the about 0.3 μ m of crystallite dimension can realize micron order processing, can guarantee the requirement of dimensional accuracy.2) zirconia material intensity height, corrosion-resistant, wear-resistant, can satisfy complicated working condition requirement, rate of wear is extremely low in the process of plug repeatedly.3) close (zirconic linear expansion coefficient is 8.3 * 10 to zirconic physical characteristics with fiber optic materials -6/ ℃, the linear expansion coefficient 5 * 10 of glass optical fiber material -6/ ℃), can realize effective coupling of optical fiber and contact pin.
Obtain the required precision of contact pin finished product, at first high-precision base substrate will be arranged.The joints of optical fibre mainly contain dry-pressing formed, extrusion forming and injection moulding with the forming method of ceramic contact pin base substrate.Dry-pressing formed apparatus and process is simple, but the dimensional accuracy of molding blank is low, and sintered body is difficult to reach even compact; Extrusion forming is that ultra-fine Zirconium powder is fully mixed with cementing agent, lubricant, make powder have certain fluidity, under certain pressure, pass through the nozzle extrusion molding, its production efficiency is higher, but the base substrate that obtains does not have the optical fiber lead-in groove, need machine work to obtain, so both improved production cost, destroy ceramic body again easily; At present most widely used is injection molding technique; being about to ceramic powder mixes with organic binder bond; make it have certain plasticity, will have the plasticity ceramic powder under certain pressure and temperature, to inject mould, treat that curing and demolding obtains the high ceramic body of dimensional accuracy.But the ceramic plasticity material viscosity used owing to injection is very big, and injection pressure and dwell pressure are very high, very easily cause fracture (Fig. 3) of metal die front end micropin, influence production efficiency, causes production cost to improve.As the ceramic contact pin Coinjection molding apparatus of Japanese pottery Co., Ltd. (Toto) invention, injection pressure is 90~180Mpa, dwell pressure 18~80Mpa, and the viscosity of ceramic raw material is 50~150Pas; The ceramic contact pin Coinjection molding apparatus of U.S. EIDU company design, injection pressure is about 136Mpa.
The colloidal state consolidation in-situ forming as gel casting forming with directly solidify casting, is a kind of in-situ solidifying forming method of ceramic size, can realize near-net-shape; Though traditional injection molding technique has the automaticity height and is easy to the advantage of large-scale production, this arts demand adds large amount of organic, and binder removal is a key issue of its widespread use of restriction all the time.The injection moulding and the colloidal formation of pottery exist huge difference, are that mainly the former belongs to the category of plastic forming, and the latter belongs to lean property sizing material forming (slurry does not have plasticity).Colloidal formation can't adopt the thinking of traditional ceramic injection forming to realize automation mechanized operation because slurry does not have plasticity.If colloidal formation combines with injection moulding, the novel curing technology that promptly utilizes proprietary injection device and colloidal state original position moulding process to be provided, the colloidal injection moulding of realization stupalith.This new technology both had been different from general colloidal formation, be different from traditional injection moulding again, it is good both to have colloidal state consolidation in-situ forming even green body, the characteristic that organic content is low, having the high advantage of injection moulding automaticity again, will be the distillation of a germplasm of colloidal formation technology.
Summary of the invention
For achieving the above object, the invention provides a kind of base substrate dimensional accuracy height that guarantees, be out of shape forming method and the device of the little joints of optical fibre with zirconium oxide ceramic contact pin.
A kind of joints of optical fibre that the present invention proposes shaped device of zirconium oxide ceramic contact pin, it is characterized in that: this device contains punch 1, guide rail 2, feeder trough 3, die 4 and the feed handle 5 that is positioned at feeder trough 3 bottoms, be positioned at the feed mouth 6 on feeder trough 3 tops, be positioned at the handle 7 at device top, be positioned at the device middle and upper part and be used to guarantee the linear bearing 8 of punch 1 running precision, be positioned at the envelope pulpboard 9 of die 4 centres, described feeder trough 3 docks with die 4, and described punch 1 can slowly at the uniform velocity move downward along guide rail 2.
In above-mentioned shaped device, the diameter of described punch 1 front end fine needle 10 is 0.15~0.18mm, and length is 16~20mm, and the right alignment of the thick handle 11 in fine needle and rear portion is less than 5 μ m; Right alignment<5 μ the m of die endoporus 12 and outer conical surface 13, the surfaceness≤Ra0.32 of endoporus 12, the quality of fit of die and punch are 5 μ m.
A kind of joints of optical fibre that the present invention proposes forming method of zirconium oxide ceramic contact pin, it is characterized in that: described method is that organic monomer and crosslinking chemical and deionized water are hybridly prepared into premixed liquid, in premixed liquid, add ceramic powder, obtain the ceramic size of viscosity<1Pas behind the ball milling, in slurry, add catalyzer and initiating agent, after mixing, inject mold cavity by molding equipment, organic monomer generation polymerization in the slip forms spacial framework, molding blank is sintering after super-dry, and its forming method carries out successively as follows:
(1) organic monomer and the crosslinking chemical that adds 10~30wt% in deionized water is mixed with premixed liquid, and wherein the weight ratio of organic monomer and crosslinking chemical is between 100: 1~25: 1;
(2) zirconia ceramics powder and organic monomer premixed liquid are mixed,, obtain the ceramic size of viscosity<1Pas through ball milling;
(3) get ceramic size,, mix the back and inject feeder trough 3 to wherein adding 0.2~0.3wt% catalyzer, 0.3~0.4wt% initiating agent;
(4) feeder trough 3 is docked with the die 4 on top, rotate feed handle 5, slurry injects die 4 by feed mouth 6;
(5) handle 7 at wheelwork top makes punch 1 slowly at the uniform velocity move down along guide rail 2, finally cooperates with die 4;
(6) be rotated further feed handle 5, make slurry pressurize in mould, the envelope of closing then pulpboard 9;
(7) treat slurry curing after, the demoulding obtains molding blank, drying;
(8) with molding blank at 1500~1550 ℃ of following sintering, obtain zirconium oxide ceramic contact pin.
In above-mentioned forming method, described organic monomer is an acrylamide, Methacrylamide, any in the methacrylic acid.
In above-mentioned forming method, described crosslinking chemical is a methylene-bisacrylamide, diallyl tartrate diamides, any in the poly dimethyl acrylic acid.
In above-mentioned forming method, described catalyzer is a tetramethylethylenediamine.
In above-mentioned forming method, described initiating agent is an ammonium persulfate, hydrogen peroxide, any in the hydrochloric acid azo.
Utilize shaped device of the present invention and method to make ceramic size can realize filling type and curing, the ceramic body even compact that is obtained, sintered body excellent performance at normal temperatures and pressures.Particularly the viscosity of this slurry very low (<1Pas), fill type and when solidifying the micropin to the punch front end do not have the side direction acting force, can not damage the punch micropin, also can not cause the skew of micropin, the requirement of mould and equipment is reduced.This method is low to mould and equipment requirements, can near-net-shape meets the joints of optical fibre zirconium oxide ceramic contact pin base substrate of dimension precision requirement.
It can accomplish the end in view evidence.
Description of drawings
Fig. 1 is a joints of optical fibre schematic diagram.
Fig. 2 is the ceramic contact pin sketch.
Fig. 3 causes the synoptic diagram that fractures of metal die greatly for injection pressure.
Fig. 4 is the punch structure synoptic diagram of forming ceramic contact pin of the present invention.
Fig. 5 is the die structural representation of forming ceramic contact pin of the present invention.
Fig. 6 is the die sectional view of forming ceramic contact pin of the present invention.
Fig. 7 is a ceramic contact pin Coinjection molding apparatus synoptic diagram of the present invention.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
The present invention adopts colloidal injection moulding technology to prepare joints of optical fibre ceramic contact pin, its principle is ceramic powder and organic monomer aqueous solution and dispersant to be made the ceramic size of low viscosity, high solid loading, add an amount of initiating agent and catalyzer then, be injected into after mixing in the mould, utilize monomer polymerization reactions to form spacial framework and the moulding ceramic body.The ceramic size of this technology can realize filling type and curing, the ceramic body even compact that is obtained, sintered body excellent performance at normal temperatures and pressures.Particularly the viscosity of this slurry very low (<1Pas), fill type and when solidifying the micropin to the punch front end do not have the side direction acting force, can not damage the punch micropin, also can not cause the skew of micropin, the requirement of mould and equipment is reduced.
The organism that colloidal injection moulding technology is used is no more than 4wt%, is beneficial to binder removal.This technology is hybridly prepared into premixed liquid with organic monomer and glue crosslinking agent and deionized water, adds the zirconia ceramics powder in premixed liquid, obtains the ceramic size of viscosity<1Pas behind the ball milling.Add catalyzer and initiating agent in ceramic size, after mixing, inject mold cavity, the organic monomer generation polymerization in the slip forms spacial framework, has promptly realized the injection moulding of lean property ceramic size at normal temperatures.
The present invention has designed the mould of moulding zirconium oxide ceramic contact pin, comprises punch and die (Fig. 4).The diameter that it is characterized in that punch front end fine needle 1 is 0.15mm, and length is 18mm, length-diameter ratio>100, and the right alignment of front end fine needle 1 and the thick handle 2 in rear portion is less than 5 μ m.Right alignment<5 μ the m of die endoporus 3 and outer conical surface 4, the surfaceness of endoporus 3 is Ra0.32, the quality of fit of die and punch is 5 μ m.
Zirconium oxide ceramic contact pin is the part of superprecision, and punch, die operate steadily relatively when guaranteeing the ceramic contact pin moulding, guarantee the dimensional accuracy and batch stability of contact pin, and the present invention has manufactured and designed a sleeve forming device (Fig. 5).This equipment is characterised in that and adopted the precision drive design, make punch 1 itself that just have the Precision Machining precision along the deviation in guide rail 2 operational processs less than 5 μ m.Can be controlled in the 10 μ m with this dimensional accuracy of equipping the zirconium oxide ceramic contact pin base substrate of preparation, can satisfy the accuracy requirement of contact pin base substrate.
The technological process of the inventive method is: batching → ball milling → fill type → pressurize → curing → demoulding → drying → sintering.Specific operation process is as follows:
[1] organic monomer and the crosslinking chemical that adds 10~30wt% in deionized water is mixed with premixed liquid, and wherein the weight ratio of organic monomer and crosslinking chemical is: 100: 1-25: between 1.
[2] zirconia ceramics powder and organic monomer premixed liquid are mixed,, obtain the ceramic size of viscosity<1Pas through 12~48 hours ball millings.
[3] get a certain amount of ceramic size,, mix the back and inject feeder trough 3 to wherein adding proper catalyst, initiating agent.
[4] feeder trough 3 is docked with the die 4 on top by feed mouth 6, rotate feed handle 5, slurry injects die 4 by feed mouth 6.
[5] rotate the handle 7 of equipping topmost, punch 1 is slowly at the uniform velocity moved down along guide rail 2, finally cooperate with die 4.Adopted in the design to slide and joined the very high linear bearing of precision 8, made punch 1 can reach 1 μ m, guaranteed that contact pin punch 1 can both insert in the die 4 exactly at every turn along the running precision in guide rail 2 moving process.
[6] be rotated further feed handle 5, make slurry pressurize 2~3 minutes in mould, dwell pressure can be 0.1~10Mpa, the envelope of closing then pulpboard 9.In this process since the ceramic size viscosity that this technology is used very low (<1Pas),, can improve its serviceable life so fill in type and the pressure maintaining period fine needle to punch tip almost without any percussive action, reduce requirement to mould.
[7] treat 5~8 minutes after, slurry curing, the demoulding obtains molding blank, put into baking oven 80 ℃ dry 12 hours down.
[8] molding blank obtains zirconium oxide ceramic contact pin 1500~1550 ℃ of following sintering 2 hours.
With this colloidal shaping method and equipment obtained by molding ceramic contact pin base substrate dimensional accuracy height, be out of shape minimum.Resulting product can satisfy the dimension precision requirement of ceramic contact pin base substrate after testing.The present invention will be further described below in conjunction with embodiment:
Embodiment 1:
With 1000 gram deionized waters, 160 gram acrylamides, 4 gram N, N '-di-2-ethylhexylphosphine oxide third rare acid amides is mixed and made into premixed liquid.With 100 gram zirconia powders is raw material, mixes ball milling 24 hours, acquisition low viscosity (<1Pas) zirconia ceramics slurry with the 40ml premixed liquid.In this slurry, add proper catalyst tetramethylethylenediamine and initiator ammonium persulfate, mix the back and inject feeder trough; Rotate the slow charging of feed handle, pressurize 2 minutes, the demoulding after treating slurry curing in 7 minutes, it is 0.136mm that base substrate is measured diameter of bore after drying, 1500 ℃ of following sintering 2 hours, the measurement diameter of bore was 0.121mm, satisfies the accuracy requirement of contact pin base substrate.Base substrate dimensional accuracy and every key property at gained contact pin goods after precision grinder processing reaches request for utilization.
Embodiment 2:
1000 gram deionized waters, 250 gram Methacrylamides, 6.25 gram diallyl tartrate diamides are mixed and made into premixed liquid.With 100 gram zirconia powders is raw material, mixes ball milling 20 hours, acquisition low viscosity (<1Pas) zirconia ceramics slurry with the 35ml premixed liquid.In this slurry, add an amount of initiating agent hydrogen peroxide, mix the back and inject feeder trough; Rotate the slow charging of feed handle, pressurize 3 minutes, the demoulding after treating slurry curing in 5 minutes, it is 0.138mm that base substrate is measured diameter of bore after drying, 1520 ℃ of following sintering 2 hours, the measurement diameter of bore was 0.119mm, satisfies the accuracy requirement of contact pin base substrate.
Embodiment 3:
1000 gram deionized waters, 110 gram methacrylic acids, 8 gram poly dimethyl acrylic acids are closed and make premixed liquid.With 100 gram zirconia powders is raw material, mixes ball milling 48 hours, acquisition low viscosity (<1Pas) zirconia ceramics slurry with the 50ml premixed liquid.In this slurry, add an amount of initiating agent hydrochloric acid azo, mix the back and inject feeder trough; Rotate the slow charging of feed handle, pressurize 2 minutes, the demoulding after treating slurry curing in 8 minutes, it is 0.135mm that base substrate is measured diameter of bore after drying, 1550 ℃ of following sintering 2 hours, the measurement diameter of bore was 0.117mm, satisfies the accuracy requirement of contact pin base substrate.

Claims (7)

1, the joints of optical fibre shaped device of zirconium oxide ceramic contact pin, it is characterized in that: this device contains punch (1), guide rail (2), feeder trough (3), die (4) and the feed handle (5) that is positioned at feeder trough (3) bottom, be positioned at the feed mouth (6) on feeder trough (3) top, be positioned at the handle (7) at device top, be positioned at the device middle and upper part and be used to guarantee the linear bearing (8) of punch (1) running precision, be positioned at the middle envelope pulpboard (9) of die (4), described feeder trough (3) docks with die (4), and described punch (1) can slowly at the uniform velocity move downward along guide rail (2).
2, according to the described shaped device of claim 1, it is characterized in that: the diameter of described punch (1) front end fine needle (10) is 0.15~0.18mm, and length is 16~20mm, and the right alignment of the thick handle in fine needle and rear portion (11) is less than 5 μ m; Right alignment<5 μ the m of die endoporus (12) and outer conical surface (13), the surfaceness≤Ra0.32 of endoporus (12), the quality of fit of die and punch are 5 μ m.
3, a kind of joints of optical fibre forming method of zirconium oxide ceramic contact pin, it is characterized in that: described method is that organic monomer and crosslinking chemical and deionized water are hybridly prepared into premixed liquid, in premixed liquid, add ceramic powder, obtain the ceramic size of viscosity<1Pas behind the ball milling, in slurry, add catalyzer and initiating agent, after mixing, inject mold cavity by molding equipment, organic monomer generation polymerization in the slip forms spacial framework, molding blank is sintering after super-dry, and its forming method carries out successively as follows:
(1) organic monomer and the crosslinking chemical that adds 10~30wt% in deionized water is mixed with premixed liquid, and wherein the weight ratio of organic monomer and crosslinking chemical is between 100: 1~25: 1;
(2) zirconia ceramics powder and organic monomer premixed liquid are mixed,, obtain the ceramic size of viscosity<1Pas through ball milling;
(3) get ceramic size,, mix the back and inject feeder trough (3) to wherein adding 0.2~0.3wt% catalyzer, 0.3~0.4wt% initiating agent;
(4) feeder trough (3) is docked with the die (4) on top, rotate feed handle (5), slurry injects die (4) by feed mouth (6);
(5) handle at wheelwork top (7) makes punch (1) slowly at the uniform velocity move down along guide rail (2), finally cooperates with die (4);
(6) be rotated further feed handle (5), make slurry pressurize in mould, the envelope of closing then pulpboard (9);
(7) treat slurry curing after, the demoulding obtains molding blank, drying;
(8) with molding blank at 1500~1550 ℃ of following sintering, obtain zirconium oxide ceramic contact pin.
4, according to the described forming method of claim 3, it is characterized in that: described organic monomer is an acrylamide, Methacrylamide, any in the methacrylic acid.
5, according to the described forming method of claim 3, it is characterized in that: described crosslinking chemical is a methylene-bisacrylamide, diallyl tartrate diamides, any in the poly dimethyl acrylic acid.
6, according to the described forming method of claim 3, it is characterized in that: described catalyzer is a tetramethylethylenediamine.
7, according to the described forming method of claim 3, it is characterized in that: described initiating agent is an ammonium persulfate, hydrogen peroxide, any in the hydrochloric acid azo.
CN 03145954 2003-07-18 2003-07-18 Forming method of zirconium oxide ceramic insertion needle for fibre-optic connector and its equipment Expired - Fee Related CN1200297C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1317105C (en) * 2004-08-20 2007-05-23 中国科学院上海技术物理研究所 Method for machining zirconia ceramic pin end-face diameter
CN100410039C (en) * 2004-12-24 2008-08-13 李元科 Extrusion molding method for ceramic pin blank tube with core and extrusion head thereof
CN102205553A (en) * 2010-03-30 2011-10-05 黄石晨信光电有限责任公司 Micro ceramic ferrule forming die
CN107952877A (en) * 2017-10-19 2018-04-24 宁波涵盛智能科技有限公司 A kind of continuous stamping die and process for stamping of optical fiber crimping set

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1317105C (en) * 2004-08-20 2007-05-23 中国科学院上海技术物理研究所 Method for machining zirconia ceramic pin end-face diameter
CN100410039C (en) * 2004-12-24 2008-08-13 李元科 Extrusion molding method for ceramic pin blank tube with core and extrusion head thereof
CN102205553A (en) * 2010-03-30 2011-10-05 黄石晨信光电有限责任公司 Micro ceramic ferrule forming die
CN102205553B (en) * 2010-03-30 2012-08-29 黄石晨信光电有限责任公司 Micro ceramic ferrule forming die
CN107952877A (en) * 2017-10-19 2018-04-24 宁波涵盛智能科技有限公司 A kind of continuous stamping die and process for stamping of optical fiber crimping set

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