CN111217652B - Composite solid propellant based on fluoropolymer modified aluminum powder and preparation method thereof - Google Patents
Composite solid propellant based on fluoropolymer modified aluminum powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a composite solid propellant based on fluoropolymer modified aluminum powder and a preparation method thereof, wherein the fluoropolymer coated aluminum powder is prepared by poly-dopamine induction, so that uniform distribution of the aluminum powder and the fluoropolymer and close contact between the aluminum powder and the fluoropolymer can be realized, and the composite has the characteristics of easily adjustable components and easily controlled reaction activity; the fluoropolymer is coated on the surface of the aluminum powder (to form the novel aluminum-based composite fuel), so that the ignition energy of the aluminum powder can be reduced, the combustion efficiency of the aluminum powder is improved, and the solid propellant adopting the aluminum-based composite fuel has the characteristics of low average particle size of combustion products, high combustion efficiency of the aluminum powder and adjustable combustion speed. The preparation method provided by the invention has the advantages that the process is simple, the structure and the composition of the modified aluminum powder particles of the final product are easy to adjust, the activity is adjustable, the combustion performance of the obtained propellant is easy to adjust and control, and the combustion efficiency is high. The cost of the raw materials is low, and the industrial production is easy to realize.
Description
Technical Field
The invention belongs to the technical field of propulsion, and relates to a composite solid propellant based on fluoropolymer modified aluminum powder and a preparation method thereof.
Background
When the aluminum-containing composite solid propellant is combusted, aluminum particles are melted and agglomerated near the combustion surface to form large-particle aluminum agglomerates, which leads to insufficient combustion of aluminum powder and further generates large-size condensed phase products (Trunov M A, Schoenitiz M, Dreizin E L.ignition of aluminum powder under differential ignition conditions [ J ]. Propellant, Explosives, Pyrotechnics, 2005, 30(1): 36-43; Hasani S, Panjoyoum, Shamanian M.non-isothermal ignition kinetic analysis of oxidation of pure aluminum powder under particulate [ J ]. oxide Met, 2014, 8(1): 299-313.). The generation of the large-size condensate increases the two-phase flow loss of the engine and reduces the specific impulse of the propellant on the one hand; on the other hand, the aluminum powder is not fully oxidized, the energy is not completely released, the combustion efficiency is reduced, and the specific impulse of the propellant is reduced. Therefore, it is very urgent to study how to improve the combustion process of aluminum powder.
Another problem faced with composite solid propellants is that: how to regulate its combustion rate. Because the composite solid propellant adopts high-activity and high-content active metal, the burning rate of the composite solid propellant is always in a higher level, which brings adverse effects on the further popularization of the composite solid propellant in large-scale application. Aiming at the problem, the burning rate of the propellant grain is regulated and controlled by changing the grain type of the propellant grain or adding an additive (an NEPE propellant burning rate inhibitor: CN201510037843.3 P.2016-08-24; an application of a low-burning rate high-energy hydroxyl propellant and alicyclic diisocyanate: CN201711405412.3 P.2018-06-05). However, these methods have disadvantages in that: 1) the burning speed of the propellant can be adjusted only within a certain range; 2) changes in the shape of the charge, excess additives, have a negative effect on the energy properties of the propellant. Therefore, the development of new regulation and control technologies to realize the regulation of the burning rate of the composite solid propellant is urgently needed.
The addition of the fluoropolymer to the solid propellant can effectively improve the combustion process of the aluminum powder. Sippel et Al added Al/PTFE complex (70/30 wt.%) in place of aluminum powder to the propellant, achieved a 66% reduction in the average Combustion product particle size (Sippel T R, Son S F, Groven L J. aluminum aggregation reduction in a composite particulate Al/PTFE particles [ J ]. Combustion and Flame 2014,161(1): 311-321.). Gaurav et al also use PTFE modified aluminum powder to achieve activation of the aluminum powder during propellant Combustion, and further achieve reduction of particle size of the propellant Combustion products and improvement of Combustion efficiency (M.G, P.A.R.Effect of mechanical activation of high specific surface area with PTFE on composite solid propellant [ J ]. Combustion and Flame,2016,166: 203-. Meanwhile, experimental research also shows that: the addition of fluoropolymers to propellants has a dramatic effect on the rate of combustion. When 10% of PTFE (polytetrafluoroethylene) based on the mass of aluminum powder is added, the burning rate of the propellant fluctuates only slightly, and when the content of PTFE is increased to 40%, the burning rate of the propellant is increased by 50%, which shows that the addition of the fluoropolymer in the propellant is expected to realize the adjustment of the burning rate of the propellant in a larger range. However, in conventional studies, a method of mechanically adding fluoropolymer or other type of oxidizer to propellant (a NEPE propellant burning rate inhibitor: CN201510037843.3[ P ] 2016-08-24; a composite solid propellant and a method of preparing the same: CN201710619515.3[ P ] 2017-12-26) has been adopted, which results in randomness and difficulty in precise control of the reaction between the oxidizer and the metal fuel, and the effect achieved is still very limited.
In the traditional research, the fluoropolymer and the aluminum powder are mostly mechanically mixed and then added into the propellant, and the defects exist in the mixing uniformity and the regulation and control accuracy of reactants.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a composite solid propellant based on fluoropolymer modified aluminum powder and a preparation method thereof. The reaction uniformity between the fluoropolymer and the aluminum powder, the combustion efficiency of the aluminum powder and the adjustable controllability of the reaction are improved. Meanwhile, the invention also provides a preparation method of the composite solid propellant based on the modified aluminum powder, the corresponding propellant grains are prepared, the average size of condensed phase products is reduced by adjusting the composition of the modified aluminum powder particles, and the problem that the combustion performance of the propellant is difficult to regulate and control is solved.
Technical scheme
A composite solid propellant based on fluoropolymer modified aluminum powder comprises aluminum powder, an oxidant, a curing agent and a plasticizer; the method is characterized in that: the aluminum powder is modified aluminum powder, the surface of the aluminum powder is coated with a layer of polydopamine, and the polydopamine is coated with fluoropolymer.
The aluminum powder is any particle size aluminum powder such as micron aluminum powder, nanometer aluminum powder and the like or the combination of aluminum powder with different particle sizes.
The method for preparing the composite solid propellant based on the fluoropolymer modified aluminum powder is characterized by comprising the following steps:
step 1: adding a buffer Tris into distilled water to enable the concentration of the buffer Tris to be 0.5-1.5 mg/mL; adding dilute hydrochloric acid to adjust the pH value to 8.5, adding dopamine, stirring for 5-15 minutes to enable the solution to be brown after partial polymerization of the dopamine, adding aluminum powder, stirring to enable the dopamine to be polymerized in situ on the surface of the aluminum powder to form a polydopamine layer, filtering and drying to obtain polydopamine-coated aluminum powder; the mass ratio of the dopamine to the aluminum powder is 1: 10-1: 1;
step 2: adding the fluoropolymer and the polydopamine-coated aluminum powder into a solvent according to the mass ratio of 5: 1-1: 20, and stirring until the fluoropolymer is completely dissolved to form a mixture;
and step 3: after the mixture is subjected to ultrasonic treatment for 5-30 minutes, slowly dripping the mixture into an anti-solvent at a constant speed to separate out a solid product; the volume ratio of the mixture to the anti-solvent is 1: 1-1: 10;
and 4, step 4: vacuum drying or suction filtering and drying the solid product to obtain Al @ fluoropolymer coated aluminum powder particles bonded on the basis of the polydopamine interface layer;
and 5: drying the Al @ fluoropolymer particles and the ammonium perchlorate AP at the temperature of 40-60 ℃ for 12-48 hours;
step 6: weighing Al @ fluoropolymer particles, an oxidant ammonium perchlorate AP, a curing agent and a plasticizer, mixing in a beaker, stirring for 30 minutes to 4 hours, and placing in a PTFE square groove; the mass ratio of the Al @ fluoropolymer particles to the oxidant ammonium perchlorate AP is 1: 4-1: 6; the HTPB content accounts for 8% -15% of the total mass; the plasticizer content is lower than 2%; the content of the curing agent is 0.1-2%;
and 7: vacuumizing until no bubbles are generated, maintaining the pressure for 30 minutes to 2 hours, and then placing the mixture into an oven for curing, wherein the curing temperature is 60 to 100 ℃, and the curing time is 2 to 7 days, so as to obtain the composite solid propellant based on the fluoropolymer modified aluminum powder.
The fluoropolymer is one or more of polyvinylidene fluoride (PVD), Polytetrafluoroethylene (PTFE), perfluoropolyether, ethylene-tetrafluoroethylene copolymer (ETFE), fluorinated ethylene propylene copolymer (FEP), perfluoroalkoxy resin (PFA), Polychlorotrifluoroethylene (PCTFE), ethylene-chlorotrifluoroethylene copolymer (ECTFE) or polyvinyl fluoride.
The solvent in the step 2 is one or more of N 'N-dimethylformamide, N' N-ethylmethylformamide, methanol, dimethyl sulfoxide, dimethyl formamide, thionyl chloride, diphenyl sulfoxide or other good solvents of fluorine polymers.
And the anti-solvent in the step 3 is one or more of ethanol, cyclohexane, distilled water or other solvents which are mutually soluble with the solvent in the step 2 but do not dissolve the fluoropolymer.
Advantageous effects
According to the composite solid propellant based on the fluoropolymer modified aluminum powder and the preparation method, the fluoropolymer coated aluminum powder is prepared by poly-dopamine induction, so that uniform distribution of the aluminum powder and the fluoropolymer and close contact between the aluminum powder and the fluoropolymer can be realized, and the composite has the characteristics of easily adjustable components and easily controlled reaction activity; the fluoropolymer is coated on the surface of the aluminum powder (to form the novel aluminum-based composite fuel), so that the ignition energy of the aluminum powder can be reduced, the combustion efficiency of the aluminum powder is improved, and the solid propellant adopting the aluminum-based composite fuel has the characteristics of low average particle size of combustion products, high combustion efficiency of the aluminum powder and adjustable combustion speed.
The preparation method provided by the invention has the advantages that the process is simple, the structure and the composition of the modified aluminum powder particles of the final product are easy to adjust, the activity is adjustable, the combustion performance of the obtained propellant is easy to adjust and control, and the combustion efficiency is high. The cost of the raw materials is low, and the industrial production is easy to realize.
Drawings
FIG. 1 is a scanning electron micrograph of a fluoropolymer-based modified aluminum powder prepared according to example 1 of the present invention.
FIG. 2 is a graph of the spectrum analysis of the fluoropolymer-based modified aluminum powder prepared in example 1 of the present invention.
Fig. 3 shows the composite solid propellants prepared in example 1(a), example 2(b) and example 3 (c).
Fig. 4 is a scanning electron micrograph of the combustion products of the fluoropolymer-modified aluminum powder-based composite solid propellant prepared in examples 1 and 2 of the present invention.
FIG. 5 the burn rate of the composite solid propellant prepared in examples 1 and 2 is compared to the burn rate of a blank formulation without the addition of PVDF.
Fig. 6 is a particle size distribution diagram of the condensed phase product of the composite solid propellant prepared in example 1, example 2, example 3, example 4 and example 5 of the present invention.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1
A composite solid propellant based on fluoropolymer modified aluminum powder and a preparation method thereof comprise the following process steps:
(1) coating polydopamine on the surface of aluminum powder: adding 0.60g of dopamine and 0.36g of Tris buffer solution (pH 8.5) into 300ml of distilled water, stirring until dopamine molecules are partially polymerized (the color is changed into brown), adding 4.0g of micron aluminum powder (1-2 microns) and stirring for 30 minutes to enable polydopamine to be polymerized in situ on the surfaces of the aluminum powder to form polydopamine layers, taking out the mixture, centrifuging, freezing and drying to obtain the polydopamine-coated aluminum powder.
(2) Mixing of aluminum powder coated with polydopamine with fluoropolymer: 0.05g PVDF was weighed into 50ml N' N-dimethylformamide, stirred until PVDF was completely dissolved (about 1 hour), 1.0g polydopamine modified aluminum powder was added, and stirred at room temperature using a magnetic stirrer until uniform mixing (2 hours).
(3) Formation of fluoropolymer coating layer: and (3) slowly and uniformly dripping the mixture into 100ml of ethanol which is magnetically stirred, and separating out PVDF.
(4) And (3) collecting a product: the product was washed with distilled water, filtered and dried in an oven to collect the product.
(5) Drying raw materials for preparing the propellant: weighing fluoropolymer modified aluminum powder and Ammonium Perchlorate (AP), and drying in an oven at 50 ℃ for 1 day.
(6) Preparation of propellant slurry: the curing agent, the plasticizer, the oxidant and the modified aluminum powder are weighed and fully stirred until the mixture is uniformly mixed (about 2 hours).
(7) Discharging air bubbles and curing: and putting the propellant slurry into a drying oven, vacuumizing for 1 hour at room temperature, maintaining the pressure for 2 hours, leveling the slurry, and curing in an oven at the temperature of 80 ℃ for 4 days.
The fluoropolymer modified aluminum powder prepared in example 1 was observed by scanning electron microscopy, and the morphology is shown in FIG. 1. The results show that the particle size and distribution of the particles in the product are uniform.
The fluoropolymer-based modified aluminum powder prepared in example 1 is subjected to energy spectrum analysis to obtain an obvious core-shell structure, and an obvious PVDF coating layer is formed on the surface of the aluminum powder, as shown in FIG. 2.
The composite solid propellant based on the fluoropolymer modified aluminum powder prepared in example 1 was photographed by a camera, and the morphology of the composite solid propellant is shown in fig. 3, the components are uniformly distributed, and no obvious pores are observed.
The condensed phase product of the composite solid propellant based on fluoropolymer modified aluminum powder prepared in example 1 was analyzed by scanning electron microscopy, and as a result, as shown in fig. 4, the PVDF modified propellant has a small-sized condensed phase product, and no significant sintering of the product was observed.
The burning rate of the composite solid propellant based on fluoropolymer modified aluminum powder prepared in example 1 was measured by a high-speed camera, and the burning rate was reduced by 39% compared with that of the blank formulation, as shown in fig. 5.
The combustion product of the fluoropolymer-modified aluminum powder-based composite solid propellant prepared in example 1 was analyzed by a laser particle sizer, and as a result, as shown in fig. 6, the average particle size of the PVDF-modified propellant combustion product was 0.47 μm.
Example 2
A composite solid propellant based on fluoropolymer modified aluminum powder and a preparation method thereof comprise the following process steps:
(1) drying raw materials for preparing the propellant: weighing the fluoropolymer, aluminum powder (1-2 mu m) and ammonium perchlorate, and drying in an oven at the drying temperature of 50 ℃ for 1 day.
(2) Preparation of propellant slurry: the curing agent, plasticizer, oxidant, and aluminum powder were weighed and mixed thoroughly (about 2 hours).
(3) Discharging air bubbles and curing: and putting the propellant slurry into a drying oven, vacuumizing for 1 hour at room temperature, maintaining the pressure for 2 hours, leveling the slurry, and curing in an oven at the temperature of 80 ℃ for 4 days.
The composite solid propellant prepared in example 2 was photographed by a camera, and the morphology thereof is shown in fig. 3, and the components were uniformly distributed without any significant pores.
The condensed phase product of the composite solid propellant prepared in example 2 was analyzed by scanning electron microscopy, and as a result, as shown in fig. 4, the particle size of the condensed phase product was larger than that of the PVDF-modified aluminum powder-based propellant.
The burning rate of the composite solid propellant prepared in example 2 was measured by a high-speed camera, and the burning rate was reduced by 52% as compared with the blank formulation, as shown in fig. 5.
The combustion product of the composite solid propellant prepared in example 2 was analyzed by a laser particle size analyzer, and as a result, as shown in fig. 6, the average particle diameter of the combustion product was 0.61 μm. The average particle size of the combustion product of example 2 was increased by 29.8% compared to the average particle size of the combustion product of example 1, indicating that the use of modified aluminum powder can substantially reduce the average particle size of the propellant combustion product.
Example 3
A composite solid propellant based on fluoropolymer modified aluminum powder and a preparation method thereof comprise the following process steps:
(1) drying raw materials for preparing the propellant: weighing aluminum powder (1-2 mu m) and ammonium perchlorate, and drying in an oven at 50 ℃ for 1 day.
(2) Preparation of propellant slurry: the curing agent, plasticizer, oxidant, and aluminum powder were weighed and mixed thoroughly (about 2 hours).
(3) Discharging air bubbles and curing: and putting the propellant slurry into a drying oven, vacuumizing for 1 hour at room temperature, maintaining the pressure for 2 hours, leveling the slurry, and curing in an oven at the temperature of 80 ℃ for 4 days.
The composite solid propellant prepared in example 3 was photographed by a camera, and the morphology thereof is shown in fig. 3, the components are uniformly distributed, and no obvious pores are observed.
The combustion products of the composite solid propellant prepared in example 3 without added PVDF were analyzed by a laser particle sizer, and as a result, the average particle size of the propellant combustion product was 0.67 μm, as shown in fig. 6. The average particle size of the combustion product of example 3 was increased by 42.6% compared to the average particle size of the condensed phase combustion product of example 1, demonstrating that the use of modified aluminum powder can substantially reduce the average particle size of the propellant combustion product.
Example 4
A composite solid propellant based on fluoropolymer modified aluminum powder and a preparation method thereof comprise the following process steps:
(1) coating polydopamine on the surface of aluminum powder: adding 0.60g of dopamine and 0.36g of Tris buffer solution (pH 8.5) into 300ml of distilled water, stirring until dopamine molecules are partially polymerized (the color is changed into brown), adding 4.0g of micron aluminum powder (20-30 mu m), stirring for 30 minutes to enable poly dopamine to grow in situ on the surface of the aluminum powder to form a poly dopamine layer, taking out the mixture, centrifuging, freezing and drying to obtain the aluminum powder with the surface uniformly coated with the poly dopamine.
(2) Mixing of aluminum powder coated with polydopamine with fluoropolymer: 0.30g PVDF was weighed into 50ml N' N-dimethylformamide, stirred until PVDF was completely dissolved (about 1 hour), 1.0g polydopamine modified aluminum powder was added, and stirred at room temperature using a magnetic stirrer until uniform mixing (2 hours).
(3) Formation of fluoropolymer coating layer: and (3) slowly and uniformly dripping the mixture into 100ml of ethanol which is magnetically stirred, and separating out PVDF.
(4) And (3) collecting a product: the product was washed with distilled water, filtered and dried in an oven to collect the product.
(5) Drying raw materials for preparing the propellant: weighing fluoropolymer modified aluminum powder and ammonium perchlorate, and drying in an oven at 50 ℃ for 1 day.
(6) Preparation of propellant slurry: the curing agent, the plasticizer, the oxidant and the modified aluminum powder are weighed and fully stirred until the mixture is uniformly mixed (about 2 hours).
(7) Discharging air bubbles and curing: and putting the propellant slurry into a drying oven, vacuumizing for 1 hour at room temperature, maintaining the pressure for 2 hours, leveling the slurry, and curing in an oven at the temperature of 80 ℃ for 4 days.
The condensed phase product of the fluoropolymer-modified aluminum powder-based composite solid propellant prepared in example 4 was analyzed by a laser particle sizer, and as a result, as shown in fig. 6, the average particle size of the PVDF-modified condensed phase product of the propellant was 0.44 μm, which is much smaller than the average particle size of the condensed phase product of the propellant using a mechanical mixture as fuel. The use of modified aluminum powder is shown to greatly reduce the average particle size of the condensed phase product of the propellant.
Example 5
A composite solid propellant based on fluoropolymer modified aluminum powder and a preparation method thereof comprise the following process steps:
(1) drying raw materials for preparing the propellant: weighing a fluoropolymer (30 mass percent of aluminum powder), aluminum powder (20-30 mu m) and ammonium perchlorate, and drying in an oven at the drying temperature of 50 ℃ for 1 day.
(2) Preparation of propellant slurry: the curing agent, plasticizer, oxidant, and aluminum powder were weighed and mixed thoroughly (about 2 hours).
(3) Discharging air bubbles and curing: and putting the propellant slurry into a drying oven, vacuumizing for 1 hour at room temperature, maintaining the pressure for 2 hours, leveling the slurry, and curing in an oven at the temperature of 80 ℃ for 4 days.
The condensed phase product of the composite solid propellant prepared in example 2 was analyzed by a laser particle sizer, and as a result, as shown in fig. 6, the average particle size of the condensed phase product was 1.07 μm.
Table 1 formulation table for each example:
Claims (4)
1. a preparation method of a composite solid propellant based on fluoropolymer modified aluminum powder comprises aluminum powder, an oxidant, a curing agent, HTPB and a plasticizer; the method is characterized in that: the aluminum powder is modified aluminum powder, the surface of the aluminum powder is coated with a layer of polydopamine, and the polydopamine is coated with fluoropolymer;
the preparation method comprises the following steps:
step 1: adding a buffer Tris into distilled water to enable the concentration of the buffer Tris to be 0.5-1.5 mg/mL; adding dilute hydrochloric acid to adjust the pH value to 8.5, adding dopamine, stirring for 5-15 minutes to enable the solution to be brown after partial polymerization of the dopamine, adding aluminum powder, stirring to enable the dopamine to be polymerized in situ on the surface of the aluminum powder to form a polydopamine layer, filtering and drying to obtain polydopamine-coated aluminum powder; the mass ratio of the dopamine to the aluminum powder is 1: 10-1: 1;
step 2: adding the fluoropolymer and the polydopamine-coated aluminum powder into a solvent according to the mass ratio of 5: 1-1: 20, and stirring until the fluoropolymer is completely dissolved to form a mixture;
and step 3: after the mixture is subjected to ultrasonic treatment for 5-30 minutes, slowly dripping the mixture into an anti-solvent at a constant speed to separate out a solid product; the volume ratio of the mixture to the anti-solvent is 1: 1-1: 10;
and 4, step 4: vacuum drying or suction filtering and drying the solid product to obtain Al @ fluoropolymer coated aluminum powder particles bonded on the basis of the polydopamine interface layer;
and 5: drying the Al @ fluoropolymer particles and the ammonium perchlorate AP at the temperature of 40-60 ℃ for 12-48 hours;
step 6: weighing Al @ fluoropolymer particles, an oxidant ammonium perchlorate AP, a curing agent and a plasticizer, mixing in a beaker, stirring for 30 minutes to 4 hours, and placing in a PTFE square groove; the mass ratio of the Al @ fluoropolymer particles to the oxidant ammonium perchlorate AP is 1: 4-1: 6; the HTPB content accounts for 8% -15% of the total mass; the plasticizer content is lower than 2%; the content of the curing agent is 0.1-2%;
and 7: vacuumizing until no bubbles are generated, maintaining the pressure for 30 minutes to 2 hours, and then placing the mixture into an oven for curing, wherein the curing temperature is 60 to 100 ℃, and the curing time is 2 to 7 days, so as to obtain the composite solid propellant based on the fluoropolymer modified aluminum powder.
2. The method for preparing the composite solid propellant based on the fluoropolymer modified aluminum powder, as claimed in claim 1, is characterized in that: the fluoropolymer is one or more of polyvinylidene fluoride (PVD), perfluoropolyether, ethylene-tetrafluoroethylene copolymer (ETFE), fluorinated ethylene-propylene copolymer (FEP), perfluoroalkoxy resin (PFA), Polychlorotrifluoroethylene (PCTFE), ethylene-chlorotrifluoroethylene copolymer (ECTFE) or polyvinyl fluoride.
3. The method for preparing the composite solid propellant based on the fluoropolymer modified aluminum powder, as claimed in claim 1, is characterized in that: the solvent in the step 2 is one or more of N 'N-dimethylformamide, N' N-ethylmethylformamide, methanol, dimethyl sulfoxide, dimethyl formamide, thionyl chloride, diphenyl sulfoxide or other good solvents of fluorine polymers.
4. The method for preparing the composite solid propellant based on the fluoropolymer modified aluminum powder, as claimed in claim 1, is characterized in that: and the anti-solvent in the step 3 is one or more of ethanol, cyclohexane, distilled water or other solvents which are mutually soluble with the solvent in the step 2 but do not dissolve the fluoropolymer.
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Inventor after: Yan Qilong Inventor after: He Wei Inventor after: Qi Xiaofei Inventor after: Liu Peijin Inventor after: He Guoqiang Inventor before: Yan Qilong Inventor before: He Wei Inventor before: Qi Xiaofei Inventor before: Liu Peijin Inventor before: He Guoqiang |