阅读说明：本技术 一种光学纤维皮料管及其制备方法和应用 (Optical fiber leather pipe and preparation method and application thereof ) 是由 王久旺 周游 王云 付杨 王叶 蔡京生 于 2020-07-17 设计创作，主要内容包括：本发明是关于一种光学纤维皮料管及其制备方法和应用,所述光学纤维皮料管从内向外依次为本体层、吸收层和氧化层；所述本体层包含第一氧化物MO和M<Sub>2</Sub>O<Sub>3</Sub>中的至少一种,所述第一氧化物MO为PbO；所述第一氧化物M<Sub>2</Sub>O<Sub>3</Sub>选自Bi<Sub>2</Sub>O<Sub>3</Sub>、Cd<Sub>2</Sub>O<Sub>3</Sub>、Sn<Sub>2</Sub>O<Sub>3</Sub>、Sb<Sub>2</Sub>O<Sub>3</Sub>和As<Sub>2</Sub>O<Sub>3</Sub>中的至少一种；所述吸收层中含有与所述本体层中相同的M元素,且所述M元素的至少一部分以单质形式存在于吸收层中；所述氧化层与所述本体层的物质组成相同。该制备方法包括：将原料皮料管在氢气环境中进行还原反应；在空气环境中,将得到的皮料管经精密退火使所述吸收层的外表面以及外表面下区域中的部分单质M被氧化,从而形成氧化层。本发明的光学纤维皮料管不仅自身对杂散光具备全角度的吸收能力,同时吸收性能较高。(The invention relates to an optical fiber leather material pipe and a preparation method and application thereof, wherein the optical fiber leather material pipe sequentially comprises a body layer, an absorption layer and an oxidation layer from inside to outside; the bulk layer comprises a first oxide MO and M 2 O 3 Said first oxide MO is PbO; the first oxide M 2 O 3 Selected from Bi 2 O 3 、Cd 2 O 3 、Sn 2 O 3 、Sb 2 O 3 And As 2 O 3 At least one of; the absorbing layer contains the same M element as the body layer, and at least one part of the M element exists in the absorbing layer in a simple substance form; said oxidation being carried outThe layer has the same material composition as the bulk layer. The preparation method comprises the following steps: carrying out reduction reaction on the raw leather pipe in a hydrogen environment; and in an air environment, precisely annealing the obtained cladding pipe to oxidize the outer surface of the absorption layer and part of the simple substance M in the area below the outer surface so as to form an oxidation layer. The optical fiber leather tube disclosed by the invention has full-angle absorption capability on stray light and has higher absorption performance.)

1. The optical fiber leather material pipe is characterized in that the optical fiber leather material pipe sequentially comprises a body layer, an absorption layer and an oxidation layer from inside to outside;

the bulk layer comprises a first oxide MO and M₂O₃Said first oxide MO is PbO; the first oxide M₂O₃Selected from Bi₂O₃、Cd₂O₃、Sn₂O₃、Sb₂O₃And As₂O₃At least one of;

the absorbing layer contains the same M element as the body layer, and at least one part of the M element exists in the absorbing layer in a simple substance form;

the oxide layer and the body layer have the same material composition.

2. The fiber optic ferrule of claim 1, wherein the ratio of the thicknesses of the body layer, the absorption layer and the oxidation layer is (2.4-2.6): (0.2-0.4): (0.15-0.2).

3. The optical fiber ferrule of claim 1, wherein the body layer further comprises a second oxide comprising SiO₂、B₂O₃、Al₂O₃、Na₂O、K₂O, BaO, CaO and ZrO₂(ii) a The body layer comprises the following components in percentage by mass:

4. the preparation method of the optical fiber leather material pipe is characterized by comprising the following steps:

a reduction step: carrying out reduction reaction on the raw leather pipe in a hydrogen environment; the raw material leather hose comprises a first oxide MO and M₂O₃Said first oxide MO is PbO; the first oxide M₂O₃Selected from Bi₂O₃、Cd₂O₃、Sn₂O₃、Sb₂O₃And As₂O₃At least one of; part of the first oxide in the outer surface of the raw material leather hose and the area below the outer surface is reduced into a simple substance M to form an absorption layer;

an oxidation step: in the air environment, the cladding pipe obtained in the step 1)

Heating from normal temperature to 500-600 ℃ for 3-4 hours, and preserving the heat for 2-3 hours,

then heating to 600-630 ℃ for 2-3 hours and preserving the heat for 2-3 hours,

heating to Tg +50 ℃ after 1-2 hours, preserving the heat for 2-3 hours,

cooling to 500-600 ℃ after 2-3 hours;

cooling to normal temperature after 10-15 hours;

so that the outer surface of the absorption layer and part of the simple substance M in the area below the outer surface are oxidized to form an oxidized layer.

5. The method of claim 4, further comprising a pre-treatment step prior to the reducing step of:

supporting the inner surface of the leather tube by a support;

vacuumizing the inner part of the leather hose until the vacuum degree is 5-20 pa; and

and sealing two ports of the leather hose by melting.

6. The optical fiber comprises a skin layer and a core layer, and is characterized in that the skin layer sequentially comprises a body layer, an absorption layer and an oxidation layer from inside to outside;

the bulk layer comprises a first oxide MO and M₂O₃Said first oxide MO is PbO; the first oxide M₂O₃Selected from Bi₂O₃、Cd₂O₃、Sn₂O₃、Sb₂O₃And As₂O₃At least one of;

the absorbing layer contains the same M element as the body layer, and at least one part of the M element exists in the absorbing layer in a simple substance form;

the oxide layer and the body layer have the same material composition.

7. The optical fiber of claim 6, wherein the ratio of the thicknesses of the bulk layer, the absorption layer and the oxide layer is (2.4-2.6): (0.2-0.4): (0.15-0.2).

8. An optical fiber bundle comprising a plurality of optical fibers according to claim 6 or 7.

9. An optical fiber image-transmitting member comprising a plurality of optical fibers according to claim 6 or 7.

10. The fiber optic image transfer element of claim 9, wherein the fiber optic image transfer element is a fiber optic faceplate or a fiber optic inverter.

11. The fiber optic image transfer element of claim 9, wherein the fiber optic image transfer element is a cone of light.

12. Night vision goggles, characterized in that they comprise an image intensifier comprising an optical fiber image-transmitting element according to claim 9 or 10.

13. An endoscope, characterized in that it comprises a fiber-optic image transmitting element according to claim 9 or 10.

14. An electronic device comprising the optical fiber image transmitting element according to any one of claims 9 to 11, wherein the electronic device is a particle detector or a signal detector.

Technical Field

The invention relates to the technical field of optical fibers, in particular to an optical fiber leather material pipe and a preparation method and application thereof.

Background

The optical fiber is a core made of transparent materials such as glass, quartz or plastic, and the outer surface of the optical fiber is provided with a transparent leather tube with low refractive index. The finished component, single fiber diameter, is typically between a few microns and tens of microns.

The optical fiber image-transmitting element (such as optical fiber panel, image inverter, light cone, etc.) is made up by using several million or even tens of millions of optical fibers whose diameter is several micrometers, and making them pass through such processes of arranging them into a rod, melting-pressing, forming and optical processing. The numerical aperture can reach 1.0, and the optical film has the characteristic of optical zero thickness. The optical fiber image transmission element is used as an important element of photoelectric enhancement equipment such as a photomultiplier tube and the like, and is widely applied to high-end equipment such as night vision instruments, medical imaging equipment, energy detection and the like and the leading-edge field.

The quality of the imaging quality of the optical fiber image transmission element mainly depends on the relative optical performance parameters such as light transmittance, contrast and the like. However, in the conventional optical fiber preparation, as shown in fig. 2, a core rod 1 ', a sheath tube 2', an absorption filament 4 'and a filling filament 3' are combined to form a fiber structure (see fig. 1); and multiple materials are finally fused and molded at the same temperature, so that a plurality of factors influencing the performance are large, a plurality of uncontrollable defects are generated, and the improvement of the optical performance of an optical fiber product is limited, which is one of the key factors restricting the development of night vision optics all the time. The leather material pipe 2 'is made of a transparent glass pipe made of a single material, and an absorption wire 4' and a filling wire 3 'are inserted between fibers, wherein the absorption wire 4' can realize the absorption of stray light 5 ', and the filling wire 3' can reduce the pore proportion. Such a structure composed of a plurality of different materials is more likely to cause defects such as dark spots, grids and the like.

Disclosure of Invention

In view of the above, the main objective of the present invention is to provide an optical fiber sheath tube and a method for manufacturing the same and an application thereof, wherein the outer surface layer of the sheath tube is reduced by a reduction treatment process to generate a dark absorption layer, and the absorption layer has stray light absorption capability; the structure of the optical fiber element is improved, the fiber composed of the original core material, the leather material and the absorption material is improved into the core material and the leather material, the optimization of the optical fiber structure is realized, the absorption effect of stray light is improved, and the optical performance of the optical fiber image transmission device is improved.

The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. According to the optical fiber leather material pipe provided by the invention, the optical fiber leather material pipe sequentially comprises a body layer, an absorption layer and an oxidation layer from inside to outside;

the bulk layer comprises a first oxide MO and M₂O₃Said first oxide MO is PbO; the first oxide M₂O₃Selected from Bi₂O₃、Cd₂O₃、Sn₂O₃、Sb₂O₃And As₂O₃At least one of;

the absorbing layer contains the same M element as the body layer, and at least one part of the M element exists in the absorbing layer in a simple substance form;

the oxide layer and the body layer have the same material composition.

The object of the present invention and the technical problem to be solved can be further achieved by the following technical solutions.

Preferably, in the optical fiber sheath tube, a ratio of thicknesses of the body layer, the absorption layer and the oxidation layer is (2.4-2.6): (0.2-0.4): (0.15-0.2).

Preferably, in the optical fiber ferrule tube, the body layer further includes a second oxide, and the second oxide includes SiO₂、B₂O₃、Al₂O₃、Na₂O、K₂O, BaO, CaO and ZrO₂(ii) a The body layer comprises the following components in percentage by mass:

the purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme. The preparation method of the optical fiber leather material pipe provided by the invention comprises the following steps:

a reduction step: carrying out reduction reaction on the raw leather pipe in a hydrogen environment; the raw material leather hose comprises a first oxide MO/M₂O₃Said first oxide MO is PbO; the first oxide M₂O₃Selected from Bi₂O₃、Cd₂O₃、Sn₂O₃、Sb₂O₃And As₂O₃At least one of; part of the first oxide in the outer surface of the raw material leather hose and the area below the outer surface is reduced into a simple substance M to form an absorption layer;

an oxidation step: in the air environment, the cladding pipe obtained in the step 1)

Heating from normal temperature to 500-600 ℃ for 3-4 hours, and preserving the heat for 2-3 hours,

then heating to 600-630 ℃ for 2-3 hours and preserving the heat for 2-3 hours,

heating to Tg +50 ℃ after 1-2 hours, preserving the heat for 2-3 hours,

cooling to 500-600 ℃ after 2-3 hours;

cooling to normal temperature after 10-15 hours;

so that the outer surface of the absorption layer and part of the simple substance M in the area below the outer surface are oxidized to form an oxidized layer.

Preferably, in the preparation method of the optical fiber sheath tube, before the reduction step, a pretreatment step is further included:

supporting the inner surface of the leather tube by a support;

vacuumizing the inner part of the leather hose until the vacuum degree is 5-20 pa; and

and sealing two ports of the leather hose by melting.

Preferably, in the preparation method of the optical fiber sheath tube, after the step 2), the method further includes: cooling the leather glass tube obtained in the step 2) to normal temperature, cutting off the seals at two ends, and dismantling and fixing.

The purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme.

The optical fiber provided by the invention comprises a skin layer and a core layer, wherein the skin layer sequentially comprises a body layer, an absorption layer and an oxidation layer from inside to outside;

the bulk layer comprises a first oxide MO and M₂O₃Said first oxide MO is PbO; the first oxide M₂O₃Selected from Bi₂O₃、Cd₂O₃、Sn₂O₃、Sb₂O₃And As₂O₃At least one of;

the absorbing layer contains the same M element as the body layer, and at least one part of the M element exists in the absorbing layer in a simple substance form;

the oxide layer and the body layer have the same material composition.

Preferably, in the optical fiber, the thickness ratio of the bulk layer, the absorption layer and the oxide layer is (2.4-2.6): (0.2-0.4): (0.15-0.2).

The purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme.

According to the present invention, an optical fiber bundle is provided, which includes a plurality of optical fibers as described above.

The purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme. According to the optical fiber image transmission element provided by the invention, the optical fiber image transmission element comprises a plurality of optical fibers.

Preferably, in the optical fiber image transmission element, the optical fiber image transmission element is an optical fiber panel or an optical fiber image inverter.

Preferably, in the aforementioned optical fiber image transmission element, the optical fiber image transmission element is a light cone.

The purpose and the problem to be solved by the invention can be realized by adopting the following technical scheme. According to the night vision goggles provided by the invention, the night vision goggles comprise the image intensifier, and the image intensifier comprises the optical fiber image transmission element.

The purpose and the problem to be solved by the invention can be realized by adopting the following technical scheme. The endoscope provided by the invention comprises the optical fiber image transmitting element.

The purpose and the problem to be solved by the invention can be realized by adopting the following technical scheme.

According to the invention, the electronic device comprises the optical fiber image transmitting element, and the electronic device is a particle detector or a signal detector.

The leather tube is subjected to reduction process treatment, so that the outer layer of the leather tube generates a gradual change absorption layer and an oxidation layer, and the defect that fusion is generated between two different materials of the leather and the absorption wire due to the fact that a single absorption wire is inserted between fibers is avoided.

Compared with the prior art, the invention has the following beneficial effects:

the optical fiber cladding tube prepared by the invention not only can simplify the integral structure of the optical fiber, but also greatly reduces the generation of light transmission defects caused by the defects of fusion interfaces of various materials in the preparation process of the optical fiber, improves the relative consistency and integrity of each optical fiber and improves the optical performance of an optical fiber image transmission device. The optical fiber leather tube not only has full-angle absorption capacity on stray light, but also has higher absorption performance. The optical fiber leather material tube has the full-angle stray light absorption capacity of 360 degrees in the circumferential direction, and the absorption angle is far higher than the absorption angle of 38.5 degrees which can be reached by the arrangement mode of single fiber peripheral absorption threads in the existing high-performance optical fiber product (the contrast of transmitted optical signals is less than 1 percent); and the light absorption layer is more uniform, so that the phenomenon of uneven surface transmittance of single fibers caused by the fact that the original absorption wire arrangement mode locally absorbs stray light is avoided. In addition, the optical fiber of the present invention can be applied to high-end equipment such as night vision instruments, medical imaging instruments, energy detection, etc., and leading edge fields.

The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.

Drawings

FIG. 1 is a schematic diagram of the internal structure of a prior art optical fiber fabrication;

FIG. 2 is a schematic view of the internal structure of the optical fiber of the present invention;

FIG. 3 is a schematic structural diagram of an optical fiber ferrule of the present invention;

FIG. 4 is a schematic structural view of a coil spring tooling of the present invention;

FIG. 5 is a schematic structural view of a fixture fixing plug according to the present invention;

FIG. 6 is a schematic structural view of the coil spring tooling of the present invention after installation;

FIG. 7 is a schematic diagram of stray light absorption of the fiber optic ferrule of the present invention;

FIG. 8 is a schematic view of a prior art arrangement of absorbent filaments in a fiber rod;

FIG. 9 is a schematic view of the absorption angle of a prior art fiber rod absorbent filament;

FIG. 10 is a graph showing a comparison of the transmittance before and after reduction in example 2 of the present invention;

FIG. 11 is a graph showing the effect of reduction duration on the transmittance of the prepared optical fiber sheath tube;

FIG. 12 is a graph showing the effect of the last incubation time on the transmittance of the prepared fiber optic sheath tube;

FIG. 13 is a graph showing a comparison of the transmittance before and after reduction of the sheath tube of optical fiber according to example 7 of the present invention;

FIG. 14 is a graph showing a comparison of the transmittance before and after reduction of the optical fiber sheath tube of example 8 of the present invention;

FIG. 15A is one of XPS plots after reduction in example 1 of the present invention;

FIG. 15B is a second XPS chart showing the reduction of example 1.

Detailed Description

To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be made on the fiber optic housing tube, its manufacturing method, its application, its specific implementation, its features and its effects according to the present invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features or characteristics of one or more embodiments may be combined in any suitable manner.

The following materials or reagents, unless otherwise specified, are all commercially available.

As shown in fig. 3, the present invention provides an optical fiber leather hose, which includes a body layer 31, the body layer 31, an absorption layer 32 and an oxidation layer 33 sequentially arranged from inside to outside; said bulk layer 31 comprising a first oxide MO and M₂O₃Said first oxide MO is PbO; the first oxide M₂O₃Selected from Bi₂O₃、Cd₂O₃、Sn₂O₃、Sb₂O₃And As₂O₃Preferably PbO and Bi₂O₃Therefore, the hydrogen reduction effect can be better after optimization, and a dark and gradually changed absorption layer is generated on the surface of the glass; the absorbing layer 32 contains the same M element as the body layer 31, and at least a part of the M element exists in the absorbing layer 32 in a simple substance form, preferably, the absorbing layer 32 contains 0.3-0.9% of the simple substance by mass of the absorbing layer 32, so that the absorbing layer 32 is preparedThe prepared optical fiber leather tube has better absorption capacity on stray light; preferably, the absorption layer 32 contains Pb and Bi, so that the absorption capability of the optical fiber leather tube to stray light is better and the absorption performance is higher; the oxide layer 33 and the bulk layer 31 have the same material composition; preferably, the absorption layer 32 contains PbO and Bi respectively₂O₃Therefore, the optical fiber leather material pipe can have better interfiber fusion effect after being optimized, and simultaneously effectively eliminates the internal stress of the glass pipe and effectively prevents the glass pipe from being burst.