CN106064820B - A kind of rodlike Yb2Si2O7Raw powder's production technology - Google Patents

A kind of rodlike Yb2Si2O7Raw powder's production technology Download PDF

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CN106064820B
CN106064820B CN201610364978.5A CN201610364978A CN106064820B CN 106064820 B CN106064820 B CN 106064820B CN 201610364978 A CN201610364978 A CN 201610364978A CN 106064820 B CN106064820 B CN 106064820B
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double salt
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CN106064820A (en
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曹丽云
雍翔
黄剑锋
李翠艳
周磊
刘锦涛
欧阳海波
费杰
吴建鹏
姚春燕
郭喜燕
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Shaanxi University of Science and Technology
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract

The invention discloses a kind of rodlike Yb2Si2O7Raw powder's production technology includes the following steps：1) Yb (NO) is taken3·6H2O is made into the solution A of a concentration of 0.05~0.1mol/L；Ethyl orthosilicate and absolute ethyl alcohol are added in solution A, mixed liquor is obtained, adds the dilute hydrochloric acid of mixeding liquid volume 1%~3%, stir, obtained solution B；2) solution B microwave hydrothermal is reacted into postcooling, wet gel, dry obtained powder A is made；By powder A preheating postcoolings, powder B is made；3) Na is taken2MoO4·2H2Grinding obtains double salt after O and NaCl is sufficiently mixed, and after powder B and double salt are mixed, is reacted at 750~800 DEG C and powder C is made；4) after powder C is dissolved in water, centrifugal treating is then washed, dry, and rodlike Yb is made2Si2O7Powder.This method is easy to operate, easy to control, and reaction efficiency is high, and the time is short, and shape can be prepared under lower temperature conditions as rodlike ytterbium silicate (Yb2Si2O7) powder.

Description

A kind of rodlike Yb2Si2O7Raw powder's production technology
Technical field
The invention belongs to technical field of material, and in particular to a kind of rodlike Yb2Si2O7Raw powder's production technology.
Background technology
With the development of aerospace cause, refractory ceramics engine components play an increasingly important role.Especially Silicon based ceramic, due to its excellent high-temperature stability, mechanical behavior under high temperature and be widely used in gas-turbine unit.But It is easily to be corroded under the conditions of the high-velocity combustion comprising high-temperature vapor, so as to cause the failure of material.And thermal boundary/ring barrier Coating (EBC) is to solve the problems, such as this effective way.
Rare earth silicate, especially ytterbium silicate (Yb2Si2O7), there is no multiphases under hot conditions to change, and has simultaneously High high-temp stability and chemical stability are good, the resistance to vapor corrosion ability of excellent high temperature and are approached with silicon based ceramic substrate Coefficient of thermal expansion and [Yan-Chun Zhou, Cen Zhao, Feng Wang, Yin-Jie the advantages that good chemical compatibility Sun,Li-Ya Zheng,Xiao-Hui Wang. Theoretical Prediction and Experimental Investigation on the Thermal and Mechanical Properties of Bulkβ- Yb2Si2O7.Journal of the American Ceramic Society,2013,96(12),3891-3900.]。
At present, related ytterbium silicate (Yb2SiO5) preparation method mainly have following three kinds：Hydro-thermal method, colloidal sol-gel method, Solid phase method etc..These preparation methods all have the advantages that its uniqueness, and hydro-thermal method is higher to equipment requirement, and reaction condition is more It is harsh；Sol-gal process preparation process is complex, and digestion time is difficult to control, and Post isothermal treatment temperature is higher；Using solid phase Method preparation temperature is very high, and there are certain impurity for reaction product.
Invention content
In order to overcome the problems of the above-mentioned prior art, the purpose of the present invention is to provide a kind of rodlike Yb2Si2O7Powder The preparation method of body, this method is easy to operate, easy to control, and reaction efficiency is high, and the time is short, can be prepared under lower temperature conditions Go out shape for rodlike ytterbium silicate (Yb2Si2O7) powder.
The present invention is to be achieved through the following technical solutions：
A kind of rodlike Yb2Si2O7Raw powder's production technology includes the following steps：
1) Yb (NO) is taken3·6H2O, it is soluble in water, it is made into the solution A of a concentration of 0.05~0.1mol/L；According to Yb (NO)3·6H2O：Ethyl orthosilicate：Absolute ethyl alcohol=1：(0.8~1.2)：The molar ratio of (2.5~4), take ethyl orthosilicate and Then ethyl orthosilicate and absolute ethyl alcohol are added in solution A, obtain mixed liquor, add mixeding liquid volume 1% by absolute ethyl alcohol ~3% dilute hydrochloric acid, stirs, obtained solution B；
2) by solution B under conditions of 300~500W, 60~100 DEG C, microwave hydrothermal reacts 1~3h, is cooled to room temperature, Wet gel is made, wet gel is dried, powder A is made；By powder A at 200~400 DEG C preheating, be cooled to room temperature, make Obtain powder B；
3) according to Na2MoO4·2H2O：NaCl=1：The mass ratio of (1~5), takes Na2MoO4·2H2O and NaCl, fully Grinding obtains double salt after mixing, according to powder B：Double salt=1：The mass ratio of (1~3), after powder B and double salt are mixed, in 750 1~3h is reacted at~800 DEG C, powder C is made；
4) after powder C is dissolved in water, centrifugal treating is then washed, dry, and rodlike Yb is made2Si2O7Powder.
A concentration of 2mol/L of the step 1) dilute hydrochloric acid.
Described stir of step 1) is to be sufficiently stirred 1~3h.
Step 2) is that solution B is placed in micro-wave diminishing pot water, and control packing ratio is 30%~50%, then by micro-wave digestion Tank is placed in progress microwave hydrothermal reaction in microwave hydrothermal instrument.
Step 2) the drying is dry 6~10h by wet gel at 60~80 DEG C.
Step 2) is that powder A is placed in crucible, and then crucible is put into Muffle furnace and carries out preheating, preheating Time is 1~3h.
Step 4) is described centrifugal under 8000~9000r/min, centrifuges 10~15min.
Step 4) the washing is successively with 3~5mol/L HNO3, respectively washing 1~3 time of distilled water and absolute ethyl alcohol.
Step 4) the drying is dry 1~3h at 60~80 DEG C.
Yb (NO) used3·6H2O, ethyl orthosilicate, Na2MoO4·2H2O and NaCl is that analysis is pure.
Compared with prior art, the present invention has technique effect beneficial below：
Rodlike Yb disclosed by the invention2Si2O7Raw powder's production technology, using microwave-hydrothermal method combination molten-salt growth method, Neng Gouxian Writing reduces synthesis reaction temperature, and digestion time is easy to control, and reaction efficiency is high, and the reaction time is short, it is easier to control crystal grain Shape and size, can reduce crystal grain reunite the phenomenon that.This method technology controlling and process is simple, and cost is relatively low, reaction process It can accurately control, by the way that the factors such as reactant ratio, dilute hydrochloric acid addition is controlled to obtain predecessor of different nature, realize Reaction product morphology controllable has prepared the higher rodlike ytterbium silicate (Yb of purity under lower temperature conditions2Si2O7) powder.
Description of the drawings
Fig. 1 present invention prepared ytterbium silicate (Yb under the conditions of embodiment 42Si2O7) powder XRD spectrum；
Fig. 2 is the present invention rodlike ytterbium silicate (Yb prepared under the conditions of embodiment 42Si2O7) powder scanning electron microscope (SEM) photo.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and It is not to limit.
Embodiment 1
A kind of rodlike Yb2Si2O7Raw powder's production technology includes the following steps：
1) commercially available analytically pure Yb (NO) is weighed3·6H2O is substantially soluble in distilled water, is configured to a concentration of 0.05mol/ The solution of L, obtained solution are denoted as solution A；
2) commercially available analytically pure ethyl orthosilicate (Si (OC are measured2H5)4), according to Yb (NO)3·6H2O:Ethyl orthosilicate： Absolute ethyl alcohol=1：0.8：The ethyl orthosilicate of measurement and absolute ethyl alcohol are added in solution A by 2.5 molar ratio, are then added Enter the 2mol/L dilute hydrochloric acid of 1% volume ratio, solution B is obtained after being sufficiently stirred 1h；
3) solution B is poured into micro-wave diminishing pot water, controls packing ratio 30%, counteracting tank is placed in microwave hydrothermal instrument, Controlled at 60 DEG C, power 300W, reaction time 3h are controlled；
4) to be cooled to after room temperature, taking-up obtains wet gel, wet gel is put into thermostatic drier, controlled at 60 DEG C, dry 6h obtains powder A；
5) it will be put into crucible after dried powder A grindings, and be placed in 200 DEG C of preheating 3h in Muffle furnace, treat certainly It is so cooled to room temperature, powder B is obtained after taking-up；
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O) and sodium chloride (NaCl), the two is sufficiently mixed Double salt is obtained after grinding, according to mass ratio Na2MoO4·2H2O:NaCl=1:1, then powder B is uniformly mixed with double salt, According to powder B：Double salt=1:1 mass ratio, is placed in Muffle furnace, controls 750 DEG C of temperature, and control time 1h obtains powder C. Powder C is centrifuged, rotating speed 8000 r/min, control time 10min are controlled, with 3mol/L HNO3, distilled water, anhydrous second Alcohol respectively washing 1 time, finally dries 3h, you can obtain rodlike Yb in 60 DEG C of electric drying oven with forced convection2Si2O7Powder.
Embodiment 2
A kind of rodlike Yb2Si2O7Raw powder's production technology includes the following steps：
1) commercially available analytically pure Yb (NO) is weighed3·6H2O is substantially soluble in distilled water, is configured to a concentration of 0.08mol/ The solution of L, obtained solution are denoted as solution A；
2) commercially available analytically pure ethyl orthosilicate (Si (OC are measured2H5)4), according to Yb (NO)3·6H2O:Ethyl orthosilicate： Absolute ethyl alcohol=1：0.9：The ethyl orthosilicate of measurement and absolute ethyl alcohol are added in solution A by 3 molar ratio, are then added in The 2mol/L dilute hydrochloric acid of 2% volume ratio, solution B is obtained after being sufficiently stirred 2h；
3) solution B is poured into micro-wave diminishing pot water, controls packing ratio 40%, counteracting tank is placed in microwave hydrothermal instrument, Controlled at 70 DEG C, power 300W, reaction time 2h are controlled；
4) to be cooled to after room temperature, taking-up obtains wet gel, wet gel is put into thermostatic drier, controlled at 70 DEG C, dry 7h obtains powder A；
5) it will be put into crucible after dried powder A grindings, and be placed in 300 DEG C of preheating 2h in Muffle furnace, treat certainly It is so cooled to room temperature, powder B is obtained after taking-up；
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O) and sodium chloride (NaCl), the two is sufficiently mixed Double salt is obtained after grinding, according to mass ratio Na2MoO4·2H2O：NaCl=1：2, then powder B is uniformly mixed with double salt, According to powder B：Double salt=1:2 mass ratio, is placed in Muffle furnace, controls 800 DEG C of temperature, and control time 2h obtains powder C. Powder C is centrifuged, rotating speed 8500r/min, control time 11min are controlled, with 4mol/L HNO3, distilled water, anhydrous second Alcohol respectively washing 2 times, finally dry 2h, you can obtain rodlike Yb in 70 DEG C of electric drying oven with forced convection2Si2O7Powder.
Embodiment 3
A kind of rodlike Yb2Si2O7Raw powder's production technology includes the following steps：
1) commercially available analytically pure Yb (NO) is weighed3·6H2O is substantially soluble in distilled water, is configured to a concentration of 0.1mol/L Solution, obtained solution is denoted as solution A；
2) commercially available analytically pure ethyl orthosilicate (Si (OC are measured2H5)4), according to Yb (NO)3·6H2O:Ethyl orthosilicate： Absolute ethyl alcohol=1：1：The ethyl orthosilicate of measurement and absolute ethyl alcohol are added in solution A, then add in 1% by 3 molar ratio The 2mol/L dilute hydrochloric acid of volume ratio, solution B is obtained after being sufficiently stirred 1h；
3) solution B is poured into micro-wave diminishing pot water, controls packing ratio 30%, counteracting tank is placed in microwave hydrothermal instrument, Controlled at 100 DEG C, power 400W, reaction time 1h are controlled；
4) to be cooled to after room temperature, taking-up obtains wet gel, wet gel is put into thermostatic drier, controlled at 80 DEG C, dry 6h obtains powder A；
5) it will be put into crucible after dried powder A grindings, and be placed in 400 DEG C of preheating 1h in Muffle furnace, treat certainly It is so cooled to room temperature, powder B is obtained after taking-up；
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O) and sodium chloride (NaCl), the two is sufficiently mixed Double salt is obtained after grinding, according to mass ratio Na2MoO4·2H2O:NaCl=1:3, then powder B is uniformly mixed with double salt, According to powder B:Double salt=1:1 mass ratio, is placed in Muffle furnace, controls 850 DEG C of temperature, and control time 3h obtains powder C. Powder C is centrifuged, rotating speed 9000r/min, control time 12min are controlled, with 5mol/L HNO3, distilled water, anhydrous second Alcohol respectively washing 3 times, finally dry 3h, you can obtain rodlike Yb in 80 DEG C of electric drying oven with forced convection2Si2O7Powder.
Embodiment 4
A kind of rodlike Yb2Si2O7Raw powder's production technology includes the following steps：
1) commercially available analytically pure Yb (NO) is weighed3·6H2O is substantially soluble in distilled water, is configured to a concentration of 0.1mol/L Solution, obtained solution is denoted as solution A；
2) commercially available analytically pure ethyl orthosilicate (Si (OC are measured2H5)4), according to Yb (NO)3·6H2O：Ethyl orthosilicate： Absolute ethyl alcohol=1:1.1:The ethyl orthosilicate of measurement and absolute ethyl alcohol are added in solution A by 3.5 molar ratio, are then added Enter the 2mol/L dilute hydrochloric acid of 2% volume ratio, solution B is obtained after being sufficiently stirred 2h；
3) solution B is poured into micro-wave diminishing pot water, controls packing ratio 40%, counteracting tank is placed in microwave hydrothermal instrument, Controlled at 90 DEG C, power 500W, reaction time 1h are controlled；
4) to be cooled to after room temperature, taking-up obtains wet gel, wet gel is put into thermostatic drier, controlled at 60 DEG C, dry 10h obtains powder A；
5) it will be put into crucible after dried powder A grindings, and be placed in 300 DEG C of preheating 2h in Muffle furnace, treat certainly It is so cooled to room temperature, powder B is obtained after taking-up；
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O) and sodium chloride (NaCl), the two is sufficiently mixed Double salt is obtained after grinding, according to mass ratio Na2MoO4·2H2O:NaCl=1:4, then powder B is uniformly mixed with double salt, According to powder B：Double salt=1:3 mass ratio, is placed in Muffle furnace, controls 800 DEG C of temperature, and control time 2h obtains powder C. Powder C is centrifuged, rotating speed 8500 r/min, control time 11min are controlled, with 5mol/L HNO3, distilled water, anhydrous second Alcohol respectively washing 2 times, finally dry 3h, you can obtain rodlike Yb in 70 DEG C of electric drying oven with forced convection2Si2O7Powder.
Referring to Fig. 1, temperature is controlled just to form ytterbium silicate crystalline phase, and diffraction maximum is bright at lower 800 DEG C as shown in XRD spectrum It is aobvious, it is consistent with PDF cards 78-1212.The reason is that because liquid phase sodium molybdate-sodium chloride double salt increases reaction composition granule Diffusion and collision probability, advantageously reduce the activation energy of reaction and the synthesis temperature of ytterbium silicate.
Referring to Fig. 2, as shown in SEM photograph, when heat treatment temperature is 800 DEG C, the ytterbium silicate powder of corynebacterium is obtained, also There is part not grow into rodlike ytterbium silicate particle.Since temperature is higher, fused salt viscosity is larger, the ytterbium silicate of a part of particle shape Mutually reunite, and grown along certain orientation under the action of sodium molybdate and sodium chloride double salt, the ytterbium silicate knot of part corynebacterium Conjunction becomes larger rod-shaped powder.
Embodiment 5
A kind of rodlike Yb2Si2O7Raw powder's production technology includes the following steps：
1) commercially available analytically pure Yb (NO) is weighed3·6H2O is substantially soluble in distilled water, is configured to a concentration of 0.1mol/L Solution, obtained solution is denoted as solution A；
2) commercially available analytically pure ethyl orthosilicate (Si (OC are measured2H5)4), according to Yb (NO)3·6H2O：Ethyl orthosilicate： Absolute ethyl alcohol=1:1.2:The ethyl orthosilicate of measurement and absolute ethyl alcohol are added in solution A by 4 molar ratio, are then added in The 2mol/L dilute hydrochloric acid of 1% volume ratio, solution B is obtained after being sufficiently stirred 1h；
3) solution B is poured into micro-wave diminishing pot water, controls packing ratio 30%, counteracting tank is placed in microwave hydrothermal instrument, Controlled at 80 DEG C, power 500W, reaction time 3h are controlled；
4) to be cooled to after room temperature, taking-up obtains wet gel, wet gel is put into thermostatic drier, controlled at 60 DEG C, dry 10h obtains powder A；
5) it will be put into crucible after dried powder A grindings, and be placed in 300 DEG C of preheating 2h in Muffle furnace, treat certainly It is so cooled to room temperature, powder B is obtained after taking-up；
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O) and sodium chloride (NaCl), the two is sufficiently mixed Double salt is obtained after grinding, according to mass ratio Na2MoO4·2H2O:NaCl=1:4, then powder B is uniformly mixed with double salt, According to powder B：Double salt=1:3 mass ratio, is placed in Muffle furnace, controls 750 DEG C of temperature, and control time 1h obtains powder C. Powder C is centrifuged, rotating speed 8000 r/min, control time 10min are controlled, with 3mol/L HNO3, distilled water, anhydrous second Alcohol respectively washing 2 times, finally dry 3h, you can obtain rodlike Yb in 60 DEG C of electric drying oven with forced convection2Si2O7Powder.
In conclusion the present invention prepared under lower temperature conditions using microwave-hydrothermal method combination molten-salt growth method it is rodlike Ytterbium silicate (Yb2Si2O7) powder, main advantage is as follows：
1st, preparation method technology controlling and process disclosed by the invention is simple, and cost is relatively low；
2nd, the reaction temperature that powder is prepared using molten-salt growth method is low and the reaction time is short；
3rd, reaction process can be controlled accurately, by the way that the factors such as reactant ratio, dilute hydrochloric acid addition is controlled to obtain difference The predecessor of property；
4th, morphology controllable is realized, has prepared the higher rodlike ytterbium silicate (Yb of purity2Si2O7) powder.

Claims (8)

1. a kind of rodlike Yb2Si2O7Raw powder's production technology, which is characterized in that include the following steps：
1) Yb (NO) is taken3·6H2O, it is soluble in water, it is made into the solution A of a concentration of 0.05~0.1mol/L；According to Yb (NO)3· 6H2O：Ethyl orthosilicate：Absolute ethyl alcohol=1：(0.8~1.2)：The molar ratio of (2.5~4) takes ethyl orthosilicate and anhydrous second Then ethyl orthosilicate and absolute ethyl alcohol are added in solution A, obtain mixed liquor, add mixeding liquid volume 1%~3% by alcohol A concentration of 2mol/L dilute hydrochloric acid, stir, obtained solution B；
2) by solution B under conditions of 300~500W, 60~100 DEG C, microwave hydrothermal reacts 1~3h, is cooled to room temperature, and is made Wet gel dries wet gel, and powder A is made；By powder A at 200~400 DEG C preheating, be cooled to room temperature, be made powder Body B；
Microwave hydrothermal reaction is that solution B is placed in micro-wave diminishing pot, and control packing ratio is 30%~50%, then by micro-wave digestion Tank, which is placed in microwave hydrothermal instrument, to be reacted；
3) according to Na2MoO4·2H2O：NaCl=1：The mass ratio of (1~5), takes Na2MoO4·2H2O and NaCl, after being sufficiently mixed Grinding obtains double salt, according to powder B：Double salt=1：The mass ratio of (1~3), after powder B and double salt are mixed, in 750~800 1~3h is reacted at DEG C, powder C is made；
4) after powder C is dissolved in water, centrifugal treating is then washed, dry, and rodlike Yb is made2Si2O7Powder.
2. rodlike Yb according to claim 12Si2O7Raw powder's production technology, which is characterized in that step 1) is described fully Stir evenly is to be sufficiently stirred 1~3h.
3. rodlike Yb according to claim 12Si2O7Raw powder's production technology, which is characterized in that the step 2) drying, It is dry 6~10h by wet gel at 60~80 DEG C.
4. rodlike Yb according to claim 12Si2O7Raw powder's production technology, which is characterized in that step 2) is by powder A It is placed in crucible, then crucible is put into Muffle furnace and carries out preheating, the preheating time is 1~3h.
5. rodlike Yb according to claim 12Si2O7Raw powder's production technology, which is characterized in that the step 4) centrifugation Formula centrifuges 10~15min under 8000~9000r/min.
6. rodlike Yb according to claim 12Si2O7Raw powder's production technology, which is characterized in that the step 4) washing It is successively with 3~5mol/L HNO3, respectively washing 1~3 time of distilled water and absolute ethyl alcohol.
7. rodlike Yb according to claim 12Si2O7Raw powder's production technology, which is characterized in that the step 4) drying It is dry 1~3h at 60~80 DEG C.
8. rodlike Yb according to claim 12Si2O7Raw powder's production technology, which is characterized in that Yb (NO) used3· 6H2O, ethyl orthosilicate, Na2MoO4·2H2O and NaCl is that analysis is pure.
CN201610364978.5A 2016-05-27 2016-05-27 A kind of rodlike Yb2Si2O7Raw powder's production technology Active CN106064820B (en)

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Publication number Priority date Publication date Assignee Title
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CN101555619A (en) * 2009-02-20 2009-10-14 陕西科技大学 Preparation method of controllable yttrium silicate nano-rod
EP3010024A1 (en) * 2013-06-12 2016-04-20 Hitachi, Ltd. Tubular body and method for manufacturing tubular body

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Title
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"Yb2Si2O7的制备及性能研究";赵岑;《中国优秀硕士全文数据库 工程科技Ⅰ辑》;20131215(第S2期);第15页，第26页，图2-8 *
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