PREPARATION METHOD FOR LOW OXYGEN CONTENT SEMICONDUCTOR CORE COMPOSITE MATERIAL OPTICAL FIBRE PREFORM

Abstract

A preparation method for a low oxygen content semiconductor core composite material optical fibre preform comprise: (1) in a nitrogen gas atmosphere glovebox, tightly packing semiconductor core raw material powder into a central hole of a cladding glass tube which is sealed at one end; and (2) performing vacuum pumping on the cladding glass tube packed with the semiconductor core raw material powder, and simultaneously sealing another end of the hot-drawn glass tube to vacuum sealing the semiconductor core raw material powder within the cladding glass tube, so as to obtain the low oxygen content semiconductor core composite material optical fibre preform. The method solves problems in the traditional optical fibre preform preparation methods such as poor packing tightness, high oxygen content in drawn fibre cores, and poor transmission performance in prepared optical fibres.

Claims

1. A preparation method for a low oxygen content semiconductor core composite material optical fibre preform, wherein the preparation method comprises the following steps of: (1) in a nitrogen gas atmosphere glovebox, tightly packing a semiconductor core raw material powder into a central hole of a cladding glass tube which is sealed at one end; and (2) performing a vacuum pumping on the cladding glass tube packed with the semiconductor core raw material powder, and simultaneously sealing another end of the glass tube by hot drawing to vacuum sealing the semiconductor core raw material powder within the cladding glass tube, so as to obtain the low oxygen content semiconductor core composite material optical fibre preform.

2. The preparation method for the low oxygen content semiconductor core composite material optical fibre preform according to claim 1, wherein, in the step (1), the semiconductor core material comprises one or more of Al, Ga, In, Si, Ge, Sn, Pb, P, As, Sb, Bi, S, Se and Te.

3. The preparation method for the low oxygen content semiconductor core composite material optical fibre preform according to claim 1, wherein, in the step (1), the cladding glass tube is any oxide glass, comprising a borosilicate glass tube.

4. The preparation method for the low oxygen content semiconductor core composite material optical fibre preform according to claim 1, wherein, in the step (1), a glass softening temperature of the cladding glass tube is higher than a melting temperature of the semiconductor core.

5. The preparation method for the low oxygen content semiconductor core composite material optical fibre preform according to claim 1, wherein, in the step (2), a vacuum pressure for the vacuum pumping ranges from 10.sup.6 Pa to 100 kPa.

6. The preparation method for the low oxygen content semiconductor core composite material optical fibre preform according to claim 1, wherein the obtained optical fibre preform is wire-drawn to obtain a low oxygen content semiconductor core composite material optical fibre, and an oxygen content in the obtained low oxygen content semiconductor core composite material optical fibre is less than 5 wt %.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0021] FIG. 1 is an X-ray diffraction comparison diagram of an InSe powder raw material, an ordinary InSe semiconductor core composite material optical fibre powder and a low oxygen content InSe semiconductor core composite material optical fibre powder in an embodiment 1;

[0022] FIG. 2a is an elemental line scanning diagram of a polished end face of the ordinary InSe semiconductor core composite material optical fibre in the embodiment 1;

[0023] FIG. 2b is an elemental line scanning diagram of a polished end face of the low oxygen content InSe semiconductor core composite material optical fibre in the embodiment 1; and

[0024] FIG. 3 is an electron probe spectrometer surface scanning diagram of the polished end face of the low oxygen content InSe semiconductor core composite material optical fibre in the embodiment 1.

DETAILED DESCRIPTION

[0025] In order to better understand the present invention, the contents of the present invention will be further illustrated below with reference to the embodiments, but the embodiments of the present invention are not limited thereto, and the process parameters not specifically described may be referred to the conventional techniques.

Embodiment 1

[0026] Preparation of an optical fibre preform having InSe semiconductor core composite material and an optical fibre having InSe semiconductor core composite material:

[0027] (1) processing and cleaning of cladding glass tube: two borosilicate glass tubes with an inner diameter of 3 mm, an outer diameter of 8 mm and a length of 20 cm were used; an original length of a blanking head was 3 cm, and the two glass tubes were heated by aligning tube walls with a butane flamer; when the borosilicate glass tube was softened, a lower end of the glass tube was sealed by hot drawing; the borosilicate glass tube with the lower end sealed was cleaned in an ultrasonic cleaner for 10 minutes using 10 vol % diluted hydrochloric acid and high-purity absolute ethanol respectively at an ultrasonic frequency of 80 Hz, and an ultrasonic power of 300 W;

[0028] (2) assembling of an ordinary optical fibre preform: in the atmosphere, In powder (4N, a melting point of 156.6 C.) raw material and Se powder (4N, a melting point of 221 C.) raw material were taken out from a vacuum package, and the precursor powder was uniformly mixed according to an atomic ratio that In:Se=4:3; the cladding glass tube with the lower end sealed was vertically placed with an opening facing upward, and the mixed powder was tightly packed into the central hole of the cladding glass tube cleaned by the step (1), then the upper opening of the cladding glass tube was sealed with clay and water glass, and marked as an ordinary optical fibre preform;

[0029] (3) packaging of low oxygen content optical fibre preform: in a nitrogen gas atmosphere glovebox, the In powder (4N) raw material and Se powder (4N) raw material were taken out from a vacuum package, and the precursor powder was uniformly mixed according to an atomic ratio that In:Se=4:3; the cladding glass tube was vertically placed with the opening facing upward, and the mixed powder was tightly packed into the central hole of the cladding glass tube cleaned by the step (1); a rubber hose of a mechanical vacuum pump (with an ultimate vacuum pressure of 10.sup.2 Pa) was butted against the cladding glass tube, and a butane flame was aligned with an upper end of the glass tube to hot-draw the upper end of the cladding glass tube while performing vacuum pumping on the cladding glass tube; an original length of a feeding head was 3 cm, and the core material was vacuum-sealed inside the cladding glass tube to prepare an optical fibre preform, and mark the prepared optical fibre preform as a low oxygen content optical fibre preform; and

[0030] (4) wire-drawing of optical fibre: the ordinary optical fibre preform and the low oxygen content optical fibre preform assembled in the step (3) were sequentially placed on a commercial wire-drawing tower; under the argon atmosphere protection, a middle portion of the ordinary optical fibre preform was heated for wire-drawing at a wire-drawing temperature of 900 C.; and in a case of no atmosphere protection, the low oxygen content optical fibre preform was directly heated for wire-drawing at a wire-drawing temperature of 900 C. .

[0031] Finally, an ordinary InSe semiconductor core composite material optical fibre and a low oxygen content InSe semiconductor core composite material optical fibre was obtained, wherein the optical fibre has a diameter of 250 m and a continuous length of more than 1 m.

[0032] FIG. 1 is an X-ray diffraction comparison diagram of an InSe (an atomic ratio is that In:Se=4:3) powder material, an ordinary InSe semiconductor core composite material optical fibre powder and an low oxygen content InSe semiconductor core composite fibre powder. It can be seen from FIG. 1 that the ordinary InSe semiconductor core composite material optical fibre contains a large amount of InSe compounds and a small amount of In elemental crystals, while the low oxygen content InSe semiconductor core composite material optical fibre contains a large amount of In.sub.4Se.sub.3 and a small amount of InSe compound crystals, indicating that a combination reaction between In and Se in the low oxygen content InSe semiconductor core composite material optical fibre is more complete.

[0033] FIG. 2a and FIG. 2b are elemental line scanning diagrams of polished end faces of the ordinary InSe semiconductor core composite material optical fibre and the low oxygen content InSe semiconductor core composite material optical fibre respectively. It can be seen from FIG. 2a and FIG. 2b that the oxygen content of the low oxygen content InSe semiconductor core composite material optical fibre is less than 5 wt %, and the element distribution thereof is stable relative to that of the ordinary InSe semiconductor core composite material optical fibre.

[0034] FIG. 3 is an electron probe spectrometer surface scanning diagram of the polished end face of the low oxygen content InSe semiconductor core composite material optical fibre (O, Si, In, Se). It can be seen from FIG. 3 that the low oxygen content InSe semiconductor core composite material optical fibre has a small amount of segregation of element In, but no core cracks, and also has an excellent circularity, indicating that continuous low oxygen content InSe core composite material optical fibre is obtained.

Embodiment 2

[0035] Preparation of a low oxygen content SnSe semiconductor core composite material optical fibre preform and a low oxygen content SnSe semiconductor core composite material optical fibre:

[0036] The preparation method is the same as that of the embodiment 1 for preparing the low oxygen content InSe semiconductor core composite material optical fibre, but differs in that: the semiconductor core raw material powder was selected from tin powder (Sn, 4N, a melting point of 118.7 C.) and selenium powder (Se, 4N, a melting point of 221 C.); for the borosilicate glass tube sealed at the lower end and having a length of 15 cm, an inner diameter of 3 mm, and an outer diameter of 8 mm, the packing powder was uniformly mixed according to an atomic ratio that Sn:Se=1:1, and tightly packed into the center hole of the cladding glass tube.

[0037] The prepared low oxygen content SnSe semiconductor core composite material optical fibre has a diameter of 200 m.

[0038] A combination reaction between Sn and Se in the low oxygen content SnSe semiconductor core composite material optical fibre is relatively complete. The low oxygen content SnSe semiconductor core composite material optical fibre has a oxygen content less than 5 wt %, and a fibre core which is a mixture of SnSe and SnSe.sub.2 with excellent high temperature thermal sensitivity, and is expected to be applied to temperature sensing.

Embodiment 3

[0039] Preparation of a low oxygen content BiTe semiconductor core composite material optical fibre preform and a low oxygen content BiTe semiconductor core composite material optical fibre:

[0040] The preparation method is the same as that of the embodiment 1 for preparing the low oxygen content InSe semiconductor core composite material optical fibre, but differs in that: the semiconductor core raw material powder was selected from a commercial P-type BiTe alloy bar, and was machined into a thin alloy bar with a length of 10 cm and a diameter of 3 mm, and a melting point of 585 C. about; the borosilicate glass tube sealed at the lower end has a length of 15 cm, an inner diameter of 3 mm, and an outer diameter of 8 mm; the machined thin alloy bar was tightly packed into the center hole of the cladding glass tube. The prepared low oxygen content BiTe semiconductor core composite material optical fibre has a diameter of 200 m. A combination reaction between Bi and Te in the low oxygen content BiTe semiconductor core composite material optical fibre is relatively complete. The low oxygen content BiTe semiconductor core composite material optical fibre has an oxygen content less than 5 wt %, and stable element distribution. A fibre core has excellent low-temperature thermoelectric properties.

[0041] The optical fibre is expected to be applied to wearable low-temperature thermoelectric material power generation devices.