一种Bi/Er/La/Al共掺L波段或C+L波段石英光纤及制备方法Bi/Er/La/Al co-doped L-band or C+L-band quartz optical fiber and preparation method thereof
技术领域Technical field
本发明属于光纤技术领域,更具体的涉及一种Bi/Er/La/Al共掺石英光纤及其制备方法。The invention belongs to the technical field of optical fibers, and more specifically relates to a Bi/Er/La/Al co-doped silica optical fiber and a preparation method thereof.
背景技术Background technique
随着光纤通信技术的快速发展,通信容量不断的增加,人们对通信的带宽、容量的需求越来越高。尤其最近几年,5G业务高速增长以及物联网与云计算的应用,在环境作用下导致互联网中网传输容量有限、带宽严重不足,甚至出现“容量危机”。因此,高可信下一代互联网的网络架构中需要具有超高速、超带宽、超大容量的通信系统。而常规的波分复用(WDM)与光纤放大器相结合的技术方案越来越显现出局限性;并且,密集波分复用(DWDM)信道间隔的不断降低,对于复用和解复用的技术难度越来越大。虽然,掺铒光纤放大器实现了光纤通信系统在C波段光中继放大,大大推动了光纤通信向全光传输方向发展,但掺铒光纤的增益带宽只有35nm,仅覆盖石英光纤低损耗窗口的有限的小部分,已不能够满足用户的需求。With the rapid development of optical fiber communication technology and the continuous increase of communication capacity, people's demand for communication bandwidth and capacity is getting higher and higher. Especially in recent years, the rapid growth of 5G services and the application of the Internet of Things and cloud computing have led to limited transmission capacity and severe bandwidth shortages in the Internet under the influence of the environment, and even a "capacity crisis" has occurred. Therefore, the network architecture of the high-credibility next-generation Internet requires a communication system with ultra-high speed, ultra-bandwidth, and ultra-large capacity. The conventional wavelength division multiplexing (WDM) and optical fiber amplifiers combined technical solutions are increasingly showing their limitations; and the continuous reduction of the DWDM channel spacing, for multiplexing and demultiplexing technologies The difficulty is getting bigger and bigger. Although the erbium-doped fiber amplifier realizes the C-band optical relay amplification of the optical fiber communication system, which greatly promotes the development of optical fiber communication in the direction of all-optical transmission, the gain bandwidth of the erbium-doped fiber is only 35nm, which only covers the limited low-loss window of the silica fiber A small part of it is no longer able to meet the needs of users.
将掺铒光纤的增益谱拓宽至L波段,可实现更多波数的复用和解复用,对超宽带光信号传送,将具有重要的应用价值。本发明基于高温掺杂改进化学气相沉积法(MCVD)和原子层沉积技术(ALD),对L波段或C+L波段增益光纤进行了大量的实验研究,实现了宽带宽,高增益,对高速光纤通信的发展与光纤传感的应用具有重要的意义。Broadening the gain spectrum of the erbium-doped fiber to the L-band can achieve more wave number multiplexing and demultiplexing, which will have important application value for ultra-wideband optical signal transmission. The present invention is based on high-temperature doping-modified chemical vapor deposition (MCVD) and atomic layer deposition (ALD). A large number of experimental studies have been carried out on L-band or C+L-band gain fibers, achieving wide bandwidth, high gain, and high-speed The development of optical fiber communication and the application of optical fiber sensing are of great significance.
发明内容Summary of the invention
本发明的目的在于根据高温掺杂改进化学气相沉积法或原子层沉积技术的优势,将氧化铋、氧化铒和氧化镧纳米材料与光纤制备相结合,提供一种Bi/Er/La/Al共掺L波段或C+L波段石英光纤及其制备方法。Bi离子与Er离子之间存在能量传递,可提高泵浦吸收效率;在掺Er光纤中加入Al元素可以提高Er的浓度,并促使Er能级进一步形成斯塔克分裂,使掺Er光纤的吸收截面和发射截面展宽,同时,本专利采用Bi/Er/La/Al四种元素共掺,选择La作为共掺杂剂,是由于其作为镧系元素中分子量最小的元素,其4f电子层没有电子。因此,La在光学上不活泼,在光通信波段没有吸收峰,对Er的吸收截面和发射截面几乎不产生影响,同时La对提高折射率有一定贡献。Er/La共掺光纤在1550nm仍然是能级
4I
13/2-
4I
15/2间跃迁。La在掺Er光纤中与其它稀土元素一样,占据Si网络体中间隙位置。当将Er元素和La元素一起掺杂进光纤芯层后,如果La离子的数量足够多,则几个La 离子包围在1个Er离子四周,增大Er离子之间的间距,避免Er离子发生团聚现象,从而实现Er离子高浓度掺杂。在高浓度掺Er光纤中,Er离子吸收泵浦光后首先在Er光纤的前端产生C波段的ASE,产生的C波段的ASE再被后端光纤中的Er离子吸收,作为二次泵浦源从而形成L波段的ASE谱。该掺杂光纤具有背景损耗低、Er离子掺杂浓度高、荧光强度强,L波段的3dB增益谱宽,增益强,且结构简单,易于产业化等特点,可用于宽带光纤通信传输和放大,对高速光纤通信的发展将具有重大的推动意义。
The purpose of the present invention is to improve the advantages of chemical vapor deposition or atomic layer deposition technology based on high-temperature doping, combining bismuth oxide, erbium oxide and lanthanum oxide nanomaterials with optical fiber preparation to provide a Bi/Er/La/Al co- L wave band or C+L wave band doped silica optical fiber and preparation method thereof. There is energy transfer between Bi ions and Er ions, which can improve pump absorption efficiency; adding Al element to Er-doped fiber can increase the concentration of Er, and promote the formation of Stark splitting of Er energy level, which makes the absorption of Er-doped fiber The cross-section and emission cross-section are broadened. At the same time, this patent adopts the co-doping of the four elements Bi/Er/La/Al, and the choice of La as the co-dopant is because it is the element with the smallest molecular weight among the lanthanides, and its 4f electron layer does not electronic. Therefore, La is optically inactive, has no absorption peak in the optical communication band, and has almost no effect on the absorption and emission cross sections of Er. At the same time, La has a certain contribution to improving the refractive index. Er / La-doped fiber at 1550nm were still level 4 I 13/2 - 4 I 15/2 transition between. La, like other rare earth elements in Er-doped fibers, occupies the gap position in the Si network. When Er element and La element are doped into the fiber core layer together, if the number of La ions is large enough, several La ions are surrounded by one Er ion to increase the distance between Er ions to avoid Er ions from occurring Agglomeration phenomenon, so as to achieve high concentration of Er ions doping. In high-concentration Er-doped fiber, after Er ions absorb the pump light, C-band ASE is first generated at the front end of the Er fiber, and the C-band ASE generated is absorbed by Er ions in the back-end fiber as the secondary pump source. Thereby forming the L-band ASE spectrum. The doped fiber has the characteristics of low background loss, high Er ion doping concentration, strong fluorescence intensity, wide 3dB gain spectrum in the L-band, strong gain, simple structure, and easy industrialization. It can be used for broadband optical fiber communication transmission and amplification. It will be of great significance to the development of high-speed optical fiber communications.
为了达到上述目的,本发明采用以下技术方案:In order to achieve the above objective, the present invention adopts the following technical solutions:
一种Bi/Er/La/Al共掺L波段或C+L波段石英光纤,包括纤芯,内包层和包层,所述纤芯是由掺杂高折射率GeO
2的石英构成,所述内包层是由Bi/Er/La/Al离子共掺材料构成,所述包层是由纯石英材料构成,所述内包层包裹纤芯并位于包层的中部。
One kind of Bi / Er / La / Al codoped L-band or C + L band quartz optical fiber comprising a core, an inner cladding and a cladding, the core is a GeO 2 doped silica constituting the high refractive index, the The inner cladding layer is composed of Bi/Er/La/Al ion co-doped material, the cladding layer is composed of pure quartz material, and the inner cladding layer wraps the core and is located in the middle of the cladding layer.
所述芯层掺杂离子为铋离子Bi
0,Bi
+,Bi
3+,Bi
5+,铒离子Er
3+,镧离子La
3+,铝离子Al
3+与提高折射率分布的二氧化锗。
The core layer doped ions are bismuth ions Bi 0 , Bi + , Bi 3+ , Bi 5+ , erbium ions Er 3+ , lanthanum ions La 3+ , aluminum ions Al 3+ and germanium dioxide with improved refractive index distribution .
所述内包层是利用高温掺杂改进化学气相沉积法或原子层沉积技术交替沉积适量的Bi/Er/La/Al共掺材料,沉积厚度为10~2000nm。The inner cladding layer is formed by alternately depositing an appropriate amount of Bi/Er/La/Al co-doped material using a high-temperature doping modified chemical vapor deposition method or an atomic layer deposition technique, and the deposition thickness is 10-2000 nm.
所述纤芯直径为5.0~20.0μm,内包层直径为8.0~50.0μm,包层直径为40.0~400.0μm。The core diameter is 5.0-20.0 μm, the inner cladding diameter is 8.0-50.0 μm, and the cladding diameter is 40.0-400.0 μm.
所述纤芯与内包层可整合为Bi/Er/La/Al共掺的芯层结构。The core and the inner cladding layer can be integrated into a Bi/Er/La/Al co-doped core layer structure.
所述芯层直径为5.0~80.0μm,包层直径为60.0~400.0μm,芯层与包层的折射率差为0.3%~5.5%之间,且包层形状为圆形、四边形、六边形或八边形。The core layer has a diameter of 5.0 to 80.0 μm, the cladding diameter is 60.0 to 400.0 μm, the refractive index difference between the core layer and the cladding layer is between 0.3% and 5.5%, and the cladding shape is circular, quadrilateral, and hexagonal. Shaped or octagonal.
所述光纤的吸收峰分别为500±40,700±20,800±20,1000±40与1480±20nm;L波段3dB荧光光谱范围为1565~1630nm之间;C+L波段3dB荧光光谱范围为1530nm~1625nm之间;增益大小为10~35dB。The absorption peaks of the optical fiber are respectively 500±40,700±20,800±20, 1000±40 and 1480±20nm; the L-band 3dB fluorescence spectrum range is between 1565 and 1630nm; the C+L-band 3dB fluorescence spectrum range is between 1530nm and 1625nm Time; the gain size is 10 ~ 35dB.
该光纤可以应用于L波段(1565-1625nm)或C+L波段(1530nm-1625nm)的有源光放大光纤,有源单偏振保持光纤,有源高阶光涡旋放大光纤(阶数2-6),光纤激光器(包括连续、脉冲与可调谐激光器),以及L波段或C+L波段的宽谱光源(包括模光纤,2-6阶少模光纤,2-6阶光涡旋光源)等。The fiber can be applied to L-band (1565-1625nm) or C+L-band (1530nm-1625nm) active optical amplifier fiber, active single polarization maintaining fiber, active high-order optical vortex amplifier fiber (order 2-6) , Fiber lasers (including continuous, pulsed and tunable lasers), and wide-spectrum light sources in the L-band or C+L band (including mode fibers, 2-6-order few-mode fibers, and 2-6-order optical vortex light sources).
一种Bi/Er/La/Al共掺L波段或C+L波段有源石英光纤的制备方法,步骤如下:A method for preparing Bi/Er/La/Al co-doped L-band or C+L-band active silica fiber, the steps are as follows:
1)利用改进化学气相沉积法,即MCVD沉积二氧化硅疏松层,并将其高温处理至半透明玻璃化状态,为包层;1) Using an improved chemical vapor deposition method, that is, MCVD to deposit a loose layer of silicon dioxide, and process it at a high temperature to a semi-transparent vitrified state, which is the cladding;
2)然后,利用MCVD高温掺杂或原子层沉积技术将氧化铋、氧化铒、氧化镧与氧化铝材料均匀沉积在包层表面,为内包层;2) Then, using MCVD high temperature doping or atomic layer deposition technology to uniformly deposit bismuth oxide, erbium oxide, lanthanum oxide and aluminum oxide materials on the surface of the cladding layer, which is the inner cladding layer;
3)沉积二氧化锗,浓度控制在1.0~15.0mol%,且将掺有二氧化锗的疏松层半玻璃化,为芯层;3) Deposition of germanium dioxide, the concentration is controlled at 1.0-15.0 mol%, and the loose layer doped with germanium dioxide is semi-vitrified to become the core layer;
4)通过重复步骤2)的循环周期来调节氧化铋、氧化铒、氧化镧与氧化铝材料的掺杂浓度与掺杂粒子分布情况;4) Adjust the doping concentration and dopant particle distribution of bismuth oxide, erbium oxide, lanthanum oxide and aluminum oxide by repeating the cycle of step 2);
5)采用MCVD高温缩棒获得光纤预制棒,最后,将掺杂光纤预制棒拉丝。5) The optical fiber preform is obtained by using the MCVD high temperature shrink rod, and finally, the doped optical fiber preform is drawn.
本发明与现有技术相比较,具有如下显而易见的实质性特点和显著优点:Compared with the prior art, the present invention has the following obvious substantive features and significant advantages:
1、Bi/Er/La/Al共掺L波段或C+L波段石英光纤可实现L波段或C+L波段的高增益宽谱放大,增益大小为15~35dB;1. Bi/Er/La/Al co-doped L-band or C+L-band quartz fiber can achieve high-gain wide-spectrum amplification in L-band or C+L-band, with a gain of 15-35dB;
2、采用高温掺杂改进化学气相沉积法或原子层沉积技术,均匀性好,掺杂浓度高,方便可行,从而得到更高品质的Bi/Er/La/Al共掺L波段或C+L波段石英光纤;2. Using high temperature doping to improve chemical vapor deposition or atomic layer deposition technology, with good uniformity, high doping concentration, convenient and feasible, so as to obtain higher quality Bi/Er/La/Al co-doped L-band or C+L Band quartz fiber;
3、结构简单、价位低廉、易于产业化,可用于宽带光纤通信传输和放大,对高速光纤通信的发展将具有重大的推动意义。3. The structure is simple, the price is low, and it is easy to industrialize. It can be used for broadband optical fiber communication transmission and amplification, and it will have great significance for the development of high-speed optical fiber communication.
附图说明Description of the drawings
图1是本发明Bi/Er/La/Al共掺L波段与C+L波段石英光纤的两种结构示意图。Fig. 1 is a schematic diagram of two structures of the Bi/Er/La/Al co-doped L-band and C+L-band silica fibers of the present invention.
其中,1-芯层,2-内包层,3-包层Among them, 1-core layer, 2-inner cladding layer, 3-cladding layer
图2是本发明在L波段的荧光光谱图。Figure 2 is the fluorescence spectrum of the present invention in the L band.
图3是本发明在C+L波段的荧光光谱图。Figure 3 is the fluorescence spectrum of the present invention in the C+L band.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明进行详细说明。The present invention will be described in detail below with reference to the drawings and specific embodiments.
实施例1Example 1
参见图1,一种Bi/Er/La/Al共掺L波段石英光纤,包括纤芯1,内包层2和包层3,纤芯1是由掺杂少量高折射率的GeO
2的二氧化硅疏松层构成,内包层2是Bi/Er/La/Al共掺离子材料构成,包层3是纯石英材料构成。首先沉积二氧化硅疏松层,并将其高温处理至半透明玻璃化状态,为包层3,其次利用原子层沉积技术将氧化铋、氧化铒与氧化镧材料均匀沉积在包层3表面,为内包层2,重复循环周期,来调节氧化铋、氧化铒与氧化镧的掺杂浓度与掺杂粒子分布情况,使沉积厚度为200nm,再沉积二氧化锗,浓度控制为5.0mol%,且将掺有二氧化锗的疏松层半玻璃化,为芯层1,最后采用MCVD高温缩棒得到光纤预制棒,放置 于拉丝塔进行拉丝,制成Bi/Er/La/Al共掺L波段石英光纤,纤芯直径为5.0μm,内包层直径为8.0μm,包层直径为120.0μm,其荧光谱如图2所示。
Refer to Figure 1, a Bi/Er/La/Al co-doped L-band silica fiber, including a core 1, an inner cladding 2 and a cladding 3. The core 1 is made of a small amount of high refractive index GeO 2 dioxide The inner cladding layer 2 is composed of Bi/Er/La/Al co-doped ion material, and the cladding layer 3 is composed of pure quartz material. First, deposit a loose layer of silicon dioxide and treat it at a high temperature to a semi-transparent vitrified state, which is the cladding layer 3. Secondly, use atomic layer deposition technology to uniformly deposit bismuth oxide, erbium oxide and lanthanum oxide materials on the surface of the cladding layer 3. Inner cladding layer 2, repeat the cycle to adjust the doping concentration of bismuth oxide, erbium oxide and lanthanum oxide and the distribution of doped particles, so that the deposition thickness is 200nm, and then germanium dioxide is deposited, the concentration is controlled to 5.0mol%, and the The loose layer doped with germanium dioxide is semi-vitrified, which is the core layer 1. Finally, the MCVD high temperature shrink rod is used to obtain the optical fiber preform, which is placed in the drawing tower for drawing to make Bi/Er/La/Al co-doped L-band silica fiber , The core diameter is 5.0 μm, the inner cladding diameter is 8.0 μm, and the cladding diameter is 120.0 μm. The fluorescence spectrum is shown in Figure 2.
实施例2Example 2
参见图1,一种Bi/Er/La/Al共掺L波段或C+L波段石英光纤,包括纤芯1,内包层2和包层3,纤芯1是由掺杂少量高折射率的GeO
2的二氧化硅疏松层构成,内包层2是Bi/Er/La/Al共掺离子材料构成,包层3是纯石英材料构成或掺杂氟离子以降低少量折射率。首先沉积二氧化硅疏松层,或掺氟的二氧化硅疏松层,并将其高温处理至半透明玻璃化状态,为包层3,其次利用MCVD高温掺杂技术将氧化铋、氧化铒与氧化镧材料均匀沉积在包层3表面,为内包层2,重复循环周期,来调节氧化铋、氧化铒与氧化镧的掺杂浓度与掺杂粒子分布情况,使沉积厚度为500nm,再沉积二氧化锗,浓度控制为3.0mol%,且将掺有二氧化锗的疏松层半玻璃化,为芯层1,其次,在沉积芯层结束将在;最后,采用MCVD高温缩棒得到光纤预制棒,放置于拉丝塔进行拉丝,制成Bi/Er/La/Al共掺L波段或C+L波段石英光纤,其特征在于纤芯直径为6.0μm,内包层直径为10.0μm,包层直径为130.0μm。
Refer to Figure 1, a Bi/Er/La/Al co-doped L-band or C+L-band silica fiber, including core 1, inner cladding 2, and cladding 3. The core 1 is doped with a small amount of high refractive index GeO 2 is composed of a loose silicon dioxide layer, the inner cladding layer 2 is composed of Bi/Er/La/Al co-doped material, and the cladding layer 3 is composed of pure quartz material or doped with fluorine ions to reduce a small amount of refractive index. First, deposit a loose layer of silicon dioxide, or a loose layer of fluorine-doped silicon dioxide, and process it at a high temperature to a semi-transparent vitrified state, which is the cladding layer 3. Secondly, use MCVD high-temperature doping technology to combine bismuth oxide, erbium oxide and oxidation The lanthanum material is uniformly deposited on the surface of the cladding layer 3, which is the inner cladding layer 2. The cycle is repeated to adjust the doping concentration of bismuth oxide, erbium oxide and lanthanum oxide and the distribution of doped particles, so that the deposition thickness is 500nm, and then the deposition of dioxide The concentration of germanium is controlled to 3.0 mol%, and the loose layer doped with germanium dioxide is semi-vitrified to become core layer 1. Secondly, the end of the deposition of the core layer will be at the end; finally, the optical fiber preform is obtained by MCVD high temperature shrinking rod, Placed in the drawing tower for wire drawing to produce Bi/Er/La/Al co-doped L-band or C+L-band silica fiber, characterized by a core diameter of 6.0μm, an inner cladding diameter of 10.0μm, and a cladding diameter of 130.0 μm.
实施例3Example 3
参见图1(b),一种Bi/Er/La/Al共掺C+L波段石英光纤,包括芯层,包层3,芯层是由掺杂少量高折射率的GeO
2的二氧化硅疏松层与Bi/Er/La共掺离子材料构成,其中,Bi/Er/La/Al共掺离子采用原子层沉积技术沉积;所述包层3是由比芯层折射率低的纯石英材料构成,最后收缩成棒拉丝。其中,Bi/Er/La/Al共掺L波段石英光纤,其特征在于纤芯直径为10.0μm,内包层直径为120.0μm,芯层与包层折射率差为0.69%,包层为圆形。该掺杂光纤通过980nm、1480nm激光器双泵浦系统泵浦后,其荧光谱如图3所示。
Refer to Figure 1(b), a Bi/Er/La/Al co-doped C+L band silica fiber, including a core layer and a cladding layer 3. The core layer is made of silica doped with a small amount of high refractive index GeO 2 The loose layer is composed of Bi/Er/La co-doped ions, wherein the Bi/Er/La/Al co-doped ions are deposited by atomic layer deposition technology; the cladding layer 3 is composed of pure quartz material with a lower refractive index than the core layer , And finally shrink into a rod drawing. Among them, the Bi/Er/La/Al co-doped L-band silica fiber is characterized in that the core diameter is 10.0μm, the inner cladding diameter is 120.0μm, the refractive index difference between the core and the cladding is 0.69%, and the cladding is circular . After the doped fiber is pumped by the 980nm, 1480nm laser dual pump system, its fluorescence spectrum is shown in Figure 3.
实施例4Example 4
参见图1(b),一种Bi/Er/La/Al共掺L波段或C+L波段石英光纤,包括芯层,包层3,芯层是由掺杂少量高折射率的GeO
2的二氧化硅疏松层与Bi/Er/La/Al共掺离子材料构成,其中,Bi/Er/La/Al共掺离子采用MCVD高温掺杂技术沉积;所述包层3是由比芯层折射率低的纯石英或掺氟的纯石英材料构成;最后,收缩成棒拉丝。其中,Bi/Er/La/Al共掺L波段或C+L波段石英光纤,其特征在于纤芯直径为12.0μm,内包层直径为130.0μm,芯层与包层折射率差为0.77%,包层为圆形。
See Figure 1(b), a Bi/Er/La/Al co-doped L-band or C+L-band silica fiber, including a core layer and a cladding layer 3. The core layer is doped with a small amount of high refractive index GeO 2 The loose layer of silicon dioxide is composed of Bi/Er/La/Al co-doped ions. Among them, Bi/Er/La/Al co-doped ions are deposited by MCVD high-temperature doping technology; the cladding layer 3 is made of a higher refractive index than the core layer. It is composed of low-grade pure quartz or fluorine-doped pure quartz material; finally, it is shrunk into a rod drawing. Among them, the Bi/Er/La/Al co-doped L-band or C+L-band silica fiber is characterized in that the core diameter is 12.0μm, the inner cladding diameter is 130.0μm, and the refractive index difference between the core layer and the cladding layer is 0.77%. The cladding is round.