CN111423109A - Preparation method of rare earth chelate feed gas for gas phase doping, rare earth doped optical fiber preform and preparation method thereof - Google Patents

Preparation method of rare earth chelate feed gas for gas phase doping, rare earth doped optical fiber preform and preparation method thereof Download PDF

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CN111423109A
CN111423109A CN202010252731.0A CN202010252731A CN111423109A CN 111423109 A CN111423109 A CN 111423109A CN 202010252731 A CN202010252731 A CN 202010252731A CN 111423109 A CN111423109 A CN 111423109A
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rare earth
earth chelate
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chelate
particles
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高聪
李好
代江云
张颖娟
沈昌乐
刘念
张立华
潘大伟
李雨薇
贺红磊
王建军
景峰
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Laser Fusion Research Center China Academy of Engineering Physics
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/02—Pretreated ingredients
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod

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Abstract

The application relates to the field of vapor deposition, in particular to a preparation method of rare earth chelate feed gas for vapor phase doping, a rare earth doped optical fiber preform and a preparation method thereof. The method comprises the following steps: and (3) contacting the carrier gas with the rare earth chelate particles to ensure that the rare earth chelate particles are in a fluidized state, and heating to ensure that the fluidized rare earth chelate particles are gradually sublimated to obtain the rare earth chelate feed gas. The rare earth chelate particles in a fluidized state have a larger contact area with the carrier gas, so that the mass transfer active surface of the rare earth chelate is increased. The concentration of the rare earth chelate in the rare earth chelate feed gas can be increased. The rare earth chelate raw material gas with the same content only needs a small amount of rare earth chelate raw material, and the rare earth chelate particles do not need to be melted into liquid, so the heating temperature can be lower than the melting point temperature, and the energy consumption is saved.

Description

Preparation method of rare earth chelate feed gas for gas phase doping, rare earth doped optical fiber preform and preparation method thereof
Technical Field
The application relates to the field of vapor deposition, in particular to a preparation method of rare earth chelate feed gas for vapor phase doping, a rare earth doped optical fiber preform and a preparation method thereof.
Background
The fiber laser instrument has the advantages of high efficiency, good beam quality, compact structure, easy heat management and the like. Rare earth doped active fibers are a key component of fiber lasers. The key link of the preparation of the rare earth doped active optical fiber is the preparation of an optical fiber preform, and various parameters of the optical fiber, including rare earth doping concentration and uniformity, fiber core loss and the like, depend on a rod making process to a great extent. The rare earth doped optical fiber preform is widely prepared by adopting the modified vapor deposition technology (MCVD). The doping methods of rare earth elements are mainly divided into two types: solution doping and gas phase doping. The rare earth chelate gas phase doping technology has gradually become a main preparation method of rare earth doped optical rods at present because of the advantages of relatively low operation temperature, high saturated vapor pressure and the like. The stable supply of the rare earth chelate raw material gas is the key for realizing stable doping, and the distribution uniformity and the process repeatability of the concentration of the rare earth element doping component of the optical rod are obviously influenced.
The supply of rare earth chelate raw material gas in the prior art has the problems of high energy consumption and low raw material utilization rate.
Disclosure of Invention
An object of the embodiments of the present application is to provide a method for preparing a rare earth chelate feed gas for gas phase doping, a rare earth doped optical fiber preform and a method for preparing the same, which aim to solve the problems of high energy consumption and low raw material utilization rate in the existing preparation of a rare earth chelate feed gas.
The first aspect of the application provides a preparation method of rare earth chelate raw material gas for gas phase doping, which mainly comprises the following steps:
and (3) contacting the carrier gas with the rare earth chelate particles to ensure that the rare earth chelate particles are in a fluidized state, and heating to ensure that the fluidized rare earth chelate particles are gradually sublimated to obtain the rare earth chelate feed gas.
The carrier gas contacts with the rare earth chelate particles to enable the rare earth chelate particles to be in a fluidized state, and the fluidized rare earth chelate particles and the carrier gas have larger contact area, so that the mass transfer active surface of the rare earth chelate is increased, and the mass transfer process is more stable. The concentration of the rare earth chelate in the rare earth chelate feed gas can be increased, and the process stability is improved. In the embodiment of the present application, the rare earth chelate particle is in a liquid state without being heated to a temperature above the melting point, and thus energy consumption can be saved.
The second aspect of the application provides a preparation method of a rare earth chelate raw material gas for gas phase doping, which mainly comprises the following steps:
and introducing a carrier gas into a fluidized bed containing rare earth chelate particles, heating to gradually sublimate the fluidized rare earth chelate particles, and then carrying out gas-solid separation to obtain the rare earth chelate feed gas mainly comprising the carrier gas and the rare earth chelate.
And the carrier gas is introduced into the fluidized bed, so that the rare earth chelate particles in the fluidized bed are in a fluidized state, and the rare earth chelate particles and the carrier gas have larger contact area, thereby increasing the mass transfer active surface of the rare earth chelate. Only a small amount of rare earth chelate raw material gas is needed for the same content of rare earth chelate raw material gas. The rare earth chelate particles are in a liquid state without being heated to a temperature above the melting point, so that energy consumption can be saved.
The third aspect of the present application provides a method for preparing a rare earth doped optical fiber preform, comprising transporting a raw material gas of a rare earth chelate provided in the first aspect of the present application or provided in the second aspect of the present application for gas phase doping to a reaction zone in a glass liner for gas phase doping, performing an oxidation reaction to form rare earth oxide particles, depositing the rare earth oxide particles on a tube wall, and forming a preparation core zone of the rare earth doped optical fiber preform together with other doping materials.
The fourth aspect of the present application provides a rare earth-doped optical fiber preform, which is manufactured by the method for manufacturing the rare earth-doped optical fiber preform of the third aspect of the present application.
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In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 shows a schematic view of a gas-liquid bubbling device;
FIG. 2 shows determining umfA flow chart of (1);
FIG. 3 shows a plant for gas-phase doping of a rare earth chelate feed gas;
FIG. 4 is a schematic diagram of a first view of the distribution plate;
fig. 5 shows a schematic diagram of a second view angle of the distribution plate.
Icon: 110-a distribution plate; 111-hood.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the prior art, the generation mode of rare earth chelate gas is mainly a gas-liquid bubbling mode.
Fig. 1 shows a schematic structural diagram of a gas-liquid bubbling device, please refer to fig. 1.
The principle of the gas-liquid bubbling type is as follows: heating the rare earth chelate raw material in the bubbler to be above the melting point of the raw material, enabling the raw material to be in a liquid state, enabling carrier gas to enter from the bottom of the bubbler through a gas distributor, taking out the chelate raw material by bubbles of the carrier gas, enabling the chelate raw material to flow into a process pipeline through a gas path, introducing the process pipeline into a liner tube, oxidizing the mixture to form rare earth oxide particles, and finally doping the rare earth oxide particles into a light rod core area.
The gas-liquid bubbling type has at least the following disadvantages:
the mass transfer interface of the bubbling type mass transfer process is positioned at the interface of the bubble and the liquid level, the total mass transfer area is very limited, and the liquid level is reduced along with consumption of chelate raw materials, the bubble generation process and the gas-liquid contact time are constantly changed, so that the mass transfer process is unstable, high-concentration steam is difficult to generate, and the realization of high-concentration doping is directly influenced. Instability in the gas-liquid mass transfer process easily causes process instability, and further influences repeatability. In addition, in order to heat the chelate raw material above its melting point for effective mass transfer, both the bubbler and the entire gas circuit must be maintained at high temperatures, typically above 200 ℃, resulting in high energy consumption and low efficiency.
The following provides a detailed description of a preparation method of a rare earth chelate raw material gas for gas phase doping, a rare earth doped optical fiber preform and a preparation method thereof according to embodiments of the present application.
The preparation method of the rare earth chelate feed gas for gas phase doping mainly comprises the following steps:
and (3) contacting the carrier gas with the rare earth chelate particles to ensure that the rare earth chelate particles are in a fluidized state, and heating to ensure that the fluidized rare earth chelate particles are gradually sublimated to obtain the rare earth chelate feed gas.
In the examples of the present application, the rare earth chelate raw gas includes a carrier gas and a rare earth chelate compound, and does not contain only a rare earth chelate compound.
The carrier gas contacts with the rare earth chelate particles to ensure that the rare earth chelate particles are in a fluidized state, and the fluidized rare earth chelate particles have larger contact area with the carrier gas, so that the mass transfer active surface of the rare earth chelate is increased, and the concentration of the rare earth chelate in the rare earth chelate feed gas can be increased.
In the embodiment of the application, the rare earth chelate particles do not need to be melted into a liquid state, so that the temperature required to be heated is not high and can be lower than the melting point temperature, and the energy consumption is saved.
In the embodiment of the application, the carrier gas is helium, and the helium has good heat transfer performance and is beneficial to sublimation of the rare earth chelate. It should be noted that in other embodiments of the present application, the carrier gas may be other gases, such as nitrogen, etc.
In some embodiments of the present application, the carrier gas further comprises heating the carrier gas to a temperature in a range of from 50 ℃ below the melting point temperature of the rare earth chelate particle to the melting point temperature of the rare earth chelate particle before contacting with the rare earth chelate particle. In other words, the maximum temperature of the carrier gas is the melting point temperature (Tm) of the rare earth chelate particles, and the minimum temperature is the melting point temperature of the rare earth chelate particles minus 50 ℃. The melting point temperature (Tm) of the rare earth chelate particles is determined according to the properties of the rare earth chelate itself.
As an example, the rare earth chelate may be: er (thd)3、Tm(thd)3、Ho(thd)3、Yb(thd)3、Ce(thd)4And the like.
Further, the temperature of the carrier gas before contacting with the rare earth chelate particles is in the range of Tm-50 ℃ to Tm, for example, Tm-50 ℃, Tm-40 ℃, Tm-30 ℃, Tm-26 ℃, Tm-13 ℃, Tm-8 ℃ or Tm and the like. Further, the temperature of the carrier gas can adjust the concentration of the rare earth chelate raw material gas, and therefore, the temperature of the carrier gas can be further adjusted according to specific needs.
It is understood that in other embodiments of the present application, the temperature of the carrier gas may not be within this range, for example, the temperature of the carrier gas may be below Tm, e.g., at ambient temperature, or above Tm.
In the examples of the present application, the temperature in the fluidized bed is in the range of 50 ℃ below the melting point temperature of the rare earth chelate particle to the melting point temperature of the rare earth chelate particle. The temperature in the fluidized bed is in the range of Tm-50 ℃ to Tm, for example, Tm-50 ℃, Tm-41 ℃, Tm-35 ℃, Tm-27 ℃, Tm-11 ℃, Tm-6 ℃ or Tm, and the like. After the rare earth chelate particles are in a fluidized state, the rare earth chelate particles are gradually sublimated into gas phase under the action of heat carried by carrier gas and heat in the fluidized bed and then mixed with the carrier gas.
It should be noted that, in other embodiments of the present application, the temperature in the fluidized bed may also be other values, and only the gradual sublimation of the rare earth chelate particles is required.
Further, in some embodiments of the present application, if the rare earth chelate particles are sublimated and the gas phase contains the particles, the solid particles can be separated by gas-solid separation.
As mentioned above, the rare earth chelate particles in the fluidized bed are in a fluidized state, and are mainly related to the particle type of the rare earth chelate particles and the carrier gas flow Q, and further, the carrier gas flow Q is related to the critical fluidization rate umfStrip out rate utAnd the diameter of the fluidized bed apparatus.
The relationship of the carrier gas flow Q is as follows:
Figure BDA0002435595890000061
in the formula: d, diameter of the fluidized bed device; u. ofmf-a critical fluidization rate; u. oft-the take-off rate.
The critical fluidization rate is calculated as follows:
Figure BDA0002435595890000062
Figure BDA0002435595890000063
in the formula: phiASphericity of the particles, deVThe equivalent volume equivalent diameter of the particles,mfcritical porosity, mu-carrier gas viscosity, rho-carrier gas density, rhop-chelate particle density. Rep-particle reynolds number.
RepCalculated as follows:
Figure BDA0002435595890000064
deV-the equivalent diameter of the equivalent surface area of the particles.
The geometry of the particles and the critical bed porosity can be estimated without data using the following empirical values:
Figure BDA0002435595890000065
FIG. 2 shows determining umfReferring to FIG. 2, u is determined according to the flowchart in FIG. 2 and equations (1) to (5)mf。
Speed of discharge utDetermination of (1):
according to the Reynolds number of the particle, the carrying-out speed has 3 subareas:
rep <2, laminar flow region:
Figure BDA0002435595890000071
2< Rep <500, transition region:
Figure BDA0002435595890000072
500<Rep<2 × 105, zone of turbulence:
Figure BDA0002435595890000073
due to the take-off speed utBefore calculation, RepIs unknown becauseThis requires calculating the take-out velocity u using a trial and error methodt。
The critical fluidization velocity u can be calculated by the eight formulas, the properties of the carrier gas and the measured data of the rare earth chelate particlesmfStrip out rate utThe velocity of the carrier gas being greater than the critical fluidization velocity umfLess than the tape-out rate utAnd (4) finishing.
In some embodiments of the present application, in order to make the finally obtained rare earth chelate raw gas more stable, the concentration of the rare earth chelate raw gas is uniform during the continuous supply. The rare earth chelate particles in the fluidized bed are in a dispersed fluidized state. The particles are uniformly dispersed in the whole fluidized bed, the bed layer is uniformly expanded along with the increase of the flow velocity, the porosity in the bed is uniformly increased, the interface on the bed layer is stable, the pressure drop is stable, and the fluctuation is very small.
In bulk fluidization, the carrier gas needs to satisfy the following formula:
Figure BDA0002435595890000074
in the formula: frmf-the number of Froude numbers,
Figure BDA0002435595890000075
alternatively, in other embodiments, the rare earth chelate particles may be polyfluidized.
The application also provides a preparation method of the rare earth chelate raw material gas for gas phase doping, which mainly comprises the following steps:
and introducing a carrier gas into a fluidized bed containing rare earth chelate particles, heating to gradually sublimate the fluidized rare earth chelate particles, and then carrying out gas-solid separation to obtain the raw material gas mainly comprising the carrier gas and the rare earth chelate.
Fig. 3 shows an apparatus for gas phase doping of a rare earth chelate feed gas, referring to fig. 3, a fluidized bed contains rare earth chelate particles, a carrier gas is introduced into the fluidized bed to make the rare earth chelate particles in a fluidized state, the fluidized rare earth chelate particles are heated to gradually sublimate, and a part of the rare earth chelate enters the gas phase from the solid phase; under the action of carrier gas, a small amount of rare earth chelate particles can be carried by the carrier gas, and then rare earth chelate raw material gas with main components including the carrier gas and the rare earth chelate is obtained through gas-solid separation.
And the carrier gas is introduced into the fluidized bed, so that the rare earth chelate particles in the fluidized bed are in a fluidized state, and the rare earth chelate particles and the carrier gas have larger contact area, thereby increasing the mass transfer area of the rare earth chelate. Only a small amount of rare earth chelate raw material gas is needed for the same content of rare earth chelate raw material gas. The rare earth chelate particles do not need to be melted into liquid, so the temperature needing to be heated can be lower than the melting point temperature, and the energy consumption is saved.
In the embodiment of the application, a distribution plate 110 is arranged in the fluidized bed to prevent rare earth chelate particles from blocking the carrier gas pipe.
Fig. 4 shows a schematic structural diagram of a first view angle of the distribution plate 110, fig. 5 shows a schematic structural diagram of a second view angle of the distribution plate 110, please refer to fig. 4 and fig. 5, the distribution plate 110 is disposed in the fluidized bed, and the distribution plate 110 is located at an end of the fluidized bed close to the carrier gas pipe, and the distribution plate 110 mainly functions to prevent the rare earth chelate particles from blocking the carrier gas pipe.
The distribution plate 110 is provided with a through hole for carrier gas to pass through and a hood 111 capable of closing the through hole, the hood 111 comprises a cover body, a connecting piece and a limiting piece, two opposite ends of the connecting piece are respectively connected with the cover body and the limiting piece, the limiting piece and the cover body are respectively positioned at two sides of the through hole, and the limiting piece is close to a carrier gas pipeline; the cover body can cover the through hole, the length of the limiting part is larger than the aperture of the through hole, and the length of the connecting piece is larger than that of the through hole.
After the carrier gas is introduced into the fluidized bed, the cover body is blown away from the through hole under the action of the carrier gas, the through hole is opened, and meanwhile, the limiting piece limits the hood 111 to prevent the hood from separating from the distribution plate 110. When the carrier gas is not introduced any more, the cover body covers the through hole under the action of self gravity, so that particles are prevented from entering the carrier gas pipeline from the through hole to be blocked.
In other embodiments of the present application, the hood 111 may have other structures, and accordingly, the distribution plate 110 may have other structures.
And after the carrier gas is introduced into the fluidized bed, sublimating part of the rare earth chelate and then introducing the sublimed rare earth chelate into a gas phase, correspondingly, carrying a small amount of particles in the gas phase, separating the particles by a gas-solid separator, and returning the solid particles to the fluidized bed, wherein the gas phase is the rare earth chelate raw material gas mainly comprising the carrier gas and the rare earth chelate.
In the embodiments of the present application, the gas-solid separator is a cyclone separator, and in other embodiments of the present application, the gas-solid separator may also adopt other gas-solid separation structures.
In some embodiments of the present application, the carrier gas is helium, and the carrier gas further comprises heating the carrier gas to a temperature within a range of 50 ℃ to Tm, such as Tm-50 ℃, Tm-41 ℃, Tm-35 ℃, Tm-27 ℃, Tm-11 ℃, Tm-6 ℃, or Tm, etc., below the melting point temperature of the rare earth chelate particles before being introduced into the fluidized bed.
Accordingly, in the examples of the present application, the temperature within the fluidized bed is within a range of from 50 ℃ below the melting point temperature of the rare earth chelate particle to the melting point temperature of the rare earth chelate particle. In other words, the temperature in the fluidized bed is in the Tm-50 ℃ to Tm range.
In other embodiments of the present application, the temperature of the carrier gas may be higher than Tm or lower than (Tm-50 ℃), and accordingly, the temperature in the fluidized bed may be higher than Tm or lower than (Tm-50 ℃); only the rare earth chelate particles need to be sublimated gradually. The rare earth chelate particles in the fluidized bed are in a fluidized state and are mainly related to the particle type of the rare earth chelate particles and the carrier gas flow Q, and correspondingly, the speed of the carrier gas is greater than the critical fluidization velocity umfLess than the tape-out rate ut。
Critical fluidization velocity umfStrip out rate utPlease refer to the eight equations and the flowchart shown in fig. 2, which are not described herein again.
Accordingly, in order to make the finally obtained rare earth chelate raw material gas more stable, the concentration of the rare earth chelate raw material gas is uniform during the continuous supply. The rare earth chelate particles in the fluidized bed are in a dispersed fluidized state.
The embodiment of the application also provides a preparation method of the rare earth doped optical fiber preform, which comprises the following steps: the rare earth chelate raw material gas prepared by the preparation method for the gas-phase doped rare earth chelate raw material gas is transported to a reaction zone in a glass lining tube, oxidation reaction is carried out to form rare earth oxide particles which are deposited on the tube wall, and the rare earth oxide particles and other doping materials form the core area of a rare earth doped optical fiber preform.
In some embodiments of the present application, the material of the liner tube is quartz glass.
Based on the above, the preparation method of the rare earth chelate feed gas can save energy consumption, and the prepared rare earth chelate feed gas has uniform concentration, so the preparation method of the rare earth doped optical fiber preform has low energy consumption, the utilization rate of the rare earth chelate particles is higher, and the cost can be reduced.
In addition, the rare earth chelate raw material is not consumed much, and usually not more than 10 g, for each rare earth-doped optical fiber preform, so the size of the fluidized bed is small. Compared with an experimental device, the production device does not need amplification, does not have amplification effect, and is very favorable for optimization of the device and process improvement.
The application also provides a rare earth doped optical fiber perform rod which is prepared by the rare earth doped optical fiber perform rod.
The doping process is stable, so that the preparation process of the rare earth doped optical fiber preform is easy and stable.
The features and properties of the present application are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a rare earth chelate feed gas for gas phase doping and a preparation method of a rare earth doped optical fiber preform.
The preparation method of the rare earth chelate raw material gas for gas phase doping mainly comprises the following steps:
placing the rare earth chelate particles in a fluidized bed, introducing helium gas at 140 ℃ into the fluidized bed, keeping the temperature in the fluidized bed at 140 ℃, and separating a gas-solid mixture output by the fluidized bed through a cyclone separator to obtain the rare earth chelate feed gas for gas phase doping.
The method for preparing the rare earth doped optical fiber preform mainly comprises the following steps:
and preparing the rare earth doped optical fiber preform by adopting the obtained rare earth chelate feed gas by adopting a vapor deposition method.
Example 2
The embodiment provides a preparation method of a rare earth chelate feed gas for gas phase doping and a preparation method of a rare earth doped optical fiber preform.
The preparation method of the rare earth chelate raw material gas for gas phase doping mainly comprises the following steps:
placing the rare earth chelate particles in a fluidized bed, introducing helium gas at 150 ℃ into the fluidized bed, keeping the temperature in the fluidized bed at 150 ℃, and separating a gas-solid mixture output by the fluidized bed through a cyclone separator to obtain the rare earth chelate feed gas for gas phase doping.
The method for preparing the rare earth doped optical fiber preform mainly comprises the following steps:
and preparing the rare earth doped optical fiber preform by adopting the obtained rare earth chelate feed gas by adopting a vapor deposition method.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A preparation method of rare earth chelate feed gas for gas phase doping is characterized by mainly comprising the following steps:
and (2) contacting a carrier gas with the rare earth chelate particles to enable the rare earth chelate particles to be in a fluidized state, and heating to enable the fluidized rare earth chelate particles to gradually sublimate to obtain the rare earth chelate feed gas.
2. The method for producing a rare earth chelate raw gas for gas-phase doping according to claim 1,
contacting the carrier gas with the rare earth chelate particles to maintain the rare earth chelate particles in a dispersed fluidized state.
3. The method for preparing a rare earth chelate raw gas for gas phase doping according to claim 1, wherein in the step of contacting a carrier gas with the rare earth chelate particle to bring the rare earth chelate particle into a fluidized state, the temperature is in the range of from 50 ℃ lower than the melting point temperature of the rare earth chelate particle to the melting point temperature of the rare earth chelate particle.
4. The method for preparing a rare earth chelate feed gas for gas phase doping according to any one of claims 1 to 3, wherein the carrier gas is helium.
5. A preparation method of rare earth chelate feed gas for gas phase doping is characterized by mainly comprising the following steps:
and introducing a carrier gas into a fluidized bed containing rare earth chelate particles, heating to gradually sublimate the fluidized rare earth chelate particles, and then carrying out gas-solid separation to obtain the rare earth chelate feed gas mainly comprising the carrier gas and the rare earth chelate.
6. The method for producing a rare earth chelate raw gas for gas phase doping according to claim 5, wherein the temperature in the fluidized bed is in the range of from 50 ℃ lower than the melting point temperature of the rare earth chelate particle to the melting point temperature of the rare earth chelate particle.
7. The method for preparing a rare earth chelate raw gas for gas phase doping according to claim 5, wherein the carrier gas and the rare earth chelate particles are in a state of bulk fluidization in the fluidized bed.
8. The method for producing a rare earth chelate raw gas for gas phase doping according to any one of claims 5 to 7, wherein the carrier gas is helium gas, and the temperature of the carrier gas is in the range of from 50 ℃ lower than the melting point temperature of the rare earth chelate particle to the melting point temperature of the rare earth chelate particle.
9. A preparation method of a rare earth doped optical fiber preform is characterized by comprising the following steps:
transporting the raw gas of rare earth chelate as prepared by the method for preparing the raw gas of rare earth chelate according to any one of claims 1 to 8 to a reaction zone in a glass liner, carrying out oxidation reaction to form rare earth oxide particles, depositing the rare earth oxide particles on the tube wall, and forming the core region of a rare earth doped optical fiber preform together with other doping materials.
10. A rare earth-doped optical fiber preform, which is manufactured by the method for manufacturing a rare earth-doped optical fiber preform of claim 9.
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