CN105777140A - Preparation method of Yb2SiO5 powder - Google Patents

Preparation method of Yb2SiO5 powder Download PDF

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CN105777140A
CN105777140A CN201610065520.XA CN201610065520A CN105777140A CN 105777140 A CN105777140 A CN 105777140A CN 201610065520 A CN201610065520 A CN 201610065520A CN 105777140 A CN105777140 A CN 105777140A
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曹丽云
雍翔
周磊
黄剑锋
李翠艳
欧阳海波
费杰
吴建鹏
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a preparation method of Yb2SiO5 powder, and belongs to the technical field of ceramic material preparation.The preparation method comprises the following steps that 1, Yb(NO)3.5H2O is taken to be dissolved in absolute ethyl alcohol to prepare a solution A with the concentration of 0.05-0.1 mol/L; 2, Si(OC2H5)4 is taken to be added into the solution A, and the materials are fully stirred to be uniform to prepare a solution B; the solution B is subjected to a solvothermal reaction at the temperature of 80 DEG C-110 DEG C and then cooled to room temperature to prepare wet gel, and after the wet gel is dried, powder A is obtained; 4, the powder A is pre-sintered at 400 DEG C and then cooled to the room temperature, and powder B is prepared; 5, the powder B and Na2MoO4.2H2O are fully mixed to be uniform and sintered at the temperature of 700 DEG C-900 DEG C, and powder C is prepared; 6, the powder C is dissolved by adding water and then subjected to centrifugal treatment, and precipitates are taken to be washed and dried to prepare the Yb2Si2O5 powder.The method is simple and efficient in technology, short in reaction time and low in temperature; the Yb2Si2O5 powder prepared through the method is controllable in morphology, high in purity and uniform in particle size.

Description

A kind of Yb2SiO5Raw powder's production technology
Technical field
The invention belongs to ceramic materials preparation technology field, be specifically related to a kind of Yb2SiO5Raw powder's production technology.
Background technology
At present, some fibre strengthens SiC ceramic composite (CMCs), such as SiC fiber reinforcement SiC ceramic matrix composite material (SiC/SiC), fibre reinforced SiC ceramic matrix composite material (C/SiC), the potentiality huge due to it and be widely used in gas-turbine unit, but, major drawback is that of this material lacks durability under the high-velocity combustion environment comprising high-temperature vapor.And thermal boundary/ring barrier coating (EBC) can effectively solve this problem.
Rare earth silicate, especially ytterbium silicate (Yb2SiO5null)，It is low that it has thermal coefficient of expansion、High high-temp stability and chemical stability are good，The resistance to vapor corrosion ability of superior high temperature，And the advantage [HaimingWen such as the thermal coefficient of expansion close with silicon based ceramic substrate and good chemical compatibility,ShaomingDong,PingHe,ZhenWang,HaijunZhou,XiangyuZhang,Sol–GelSynthesisandCharacterizationofYtterbiumSilicatePowders[J].CommunicationsoftheAmericanCeramicSociety,2007,90(12):4043-4046.].Due to ytterbium silicate (Yb2SiO5) physical and chemical performance of construction features that material self possesses and a series of excellence, be therefore commonly used for thermal boundary/ring barrier material [He Shimei, Xiong Xiang, what is favorable to the people. novel Yb2SiO51400 DEG C of oxidation behaviors [J] of Environmental Barrier Coatings on Si-based Ceramics. material engineering, 2015,43 (4): 37-41.].
At present, relevant ytterbium silicate (Yb2SiO5) preparation method mainly have following three kinds: sol-gel process, solid phase method, hydro-thermal method etc..These preparation methoies all have an advantage of its uniqueness, but weak point be mostly in that complicated process of preparation, reaction time length, reaction condition requirement is harsher, need later stage Crystallizing treatment etc..
Summary of the invention
It is an object of the invention to provide a kind of Yb2SiO5Raw powder's production technology, the method technique is simple, efficient, and the response time is short, temperature is low；Through the Yb that the method prepares2SiO5Morphology microstructure is controlled, purity is high, homogeneous grain diameter.
The present invention is achieved through the following technical solutions:
The invention discloses a kind of Yb2SiO5Raw powder's production technology, comprises the following steps:
1) Yb (NO) is taken3·5H2O, is dissolved in dehydrated alcohol, is configured to the solution A that concentration is 0.05～0.1mol/L；
2) by Yb (NO)3·5H2O: tetraethyl orthosilicate=1:(0.5～0.8) mol ratio, take Si (OC2H5)4, join in solution A, stir, obtained solution B；
3) solution B is carried out at 80～110 DEG C solvent thermal reaction, be subsequently cooled to room temperature, prepare wet gel, wet gel is dried, obtain powder body A；
4) by powder body A first pre-burning at 400 DEG C, it is cooled to room temperature, prepares powder body B；
5) by powder body B:Na2MoO4·2H2O=1:(1～2) mass ratio, by powder body B and Na2MoO4·2H2O is sufficiently mixed uniformly, sinters at 700～900 DEG C, prepares powder body C；
6), after powder body C being dissolved in water, be centrifuged separating, take precipitation, by after washing of precipitate, dry, prepare Yb2SiO5Powder body.
By Si (OC2H5)4Join and solution A is sufficiently stirred for 1～3h.
Step 3) it is that solution B is placed in hydrothermal reaction kettle, reactor is placed in constant temperature oven and carries out solvent thermal reaction.
The time of solvent thermal reaction is 12～24h.
Step 3) it is that wet gel is placed in thermostatic drier, at 60～80 DEG C, dry 6～10h.
Step 4) in, to put in crucible after powder body A is ground, then crucible is placed in Muffle furnace and carries out pre-burning, the preheating time is 0.5～1h.
Step 5) in, by powder body B and Na2MoO4·2H2O is sufficiently mixed after uniformly, is placed in Muffle furnace and is sintered, and sintering time is 3～5h.
Step 6) in, it is that precipitation is used distilled water, absolute ethanol washing 3～5 times successively.
Step 6) described in centrifugal be when 8000～1000r/min, process 8～12min.
Step 6) described in dry be dry 1～3h in the electric drying oven with forced convection of 60～80 DEG C.
Compared with prior art, the present invention has following useful technique effect:
Ytterbium silicate (Yb disclosed by the invention2SiO5) raw powder's production technology, non-hydrolytic sol-gel method is adopted to be prepared in conjunction with molten-salt growth method, first at 80～110 DEG C, carry out solvent thermal reaction, prepare wet gel, after dried for wet gel powder body sequentially passes through pre-burning and 700～900 DEG C of sintering processes of 400 DEG C, the powder body C prepared is fused salt and Yb2SiO5Mixture, be dissolved in water removal fused salt after, process by centrifugation, prepare Yb2SiO5Powder body.The present invention can significantly reduce reaction temperature, shortening the response time, course of reaction can accurately control, and obtains gel of different nature by controlling the factor such as presoma, solvent, product morphology is controlled, prepares purity height, crystal development is complete, granularity is comparatively homogeneous ytterbium silicate (Yb2SiO5) powder body.The method technique is relatively easy, efficient, less costly, preparation temperature is low.
Accompanying drawing explanation
Fig. 1 is the ytterbium silicate (Yb of the embodiment of the present invention 5 preparation2SiO5) powder body XRD figure spectrum；
Fig. 2 is the ytterbium silicate (Yb of the embodiment of the present invention 5 preparation2SiO5) scanning electron microscope (SEM) photo of powder body.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Embodiment 1
A kind of Yb2SiO5Raw powder's production technology, comprises the following steps:
1) analytically pure Yb (NO) is weighed3·5H2O, is substantially soluble in dehydrated alcohol, is configured to the solution that concentration is 0.05mol/L, and the solution obtained is designated as solution A.
2) analytically pure tetraethyl orthosilicate (Si (OC is measured2H5)4), according to Yb (NO)3·5H2O: the mol ratio of tetraethyl orthosilicate=1:0.5, joins in solution A by the tetraethyl orthosilicate measured, and obtains solution B after being sufficiently stirred for 1h.
3) pouring in hydrothermal reaction kettle by solution B, be placed in constant temperature oven by reactor, controlling temperature is 80 DEG C, and the response time is 12h.
4) to be cooled after room temperature, take out and obtain wet gel, wet gel is put in thermostatic drier, controlling temperature is 60 DEG C, dry 6h, obtains powder body A.
5) dried powder body A is ground after put in crucible, be placed in Muffle furnace 400 DEG C of preheating 0.5h, after naturally cool to room temperature, after taking-up, obtain powder body B.
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O), by powder body B and Sodium Molybdate Dihydrate Homogeneous phase mixing, according to powder body B:Na2MoO4·2H2The mass ratio of O=1:1, is placed in Muffle furnace, controls temperature 900 DEG C, controls time 3h, obtains powder body C.By powder body C under 8000r/min, centrifugation 10min, collect precipitation, precipitation priority distilled water and dehydrated alcohol are each washed 3 times, finally dry 3h in the electric drying oven with forced convection of 60 DEG C, can obtain Yb2SiO5Powder body.
Embodiment 2
A kind of Yb2SiO5Raw powder's production technology, comprises the following steps:
1) analytically pure Yb (NO) is weighed3·5H2O, is substantially soluble in dehydrated alcohol, is configured to the solution that concentration is 0.1mol/L, and the solution obtained is designated as solution A.
2) analytically pure tetraethyl orthosilicate (Si (OC is measured2H5)4), according to Yb (NO)3·5H2O: the mol ratio of tetraethyl orthosilicate=1:0.6, joins in solution A by the tetraethyl orthosilicate measured, and obtains solution B after being sufficiently stirred for 2h.
3) pouring in hydrothermal reaction kettle by solution B, be placed in constant temperature oven by reactor, controlling temperature is 90 DEG C, and the response time is 12h.
4) to be cooled after room temperature, take out and obtain wet gel, wet gel is put in thermostatic drier, controlling temperature is 70 DEG C, dry 7h, obtains powder body A.
5) dried powder body A is ground after put in crucible, be placed in Muffle furnace 400 DEG C of preheating 0.5h, after naturally cool to room temperature, after taking-up, obtain powder body B.
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O), by powder body B and Sodium Molybdate Dihydrate Homogeneous phase mixing, according to powder body B:Na2MoO4·2H2The mass ratio of O=1:1.5, is placed in Muffle furnace, controls temperature 850 DEG C, controls time 3h, obtains powder body C.By powder body C under 9000r/min, centrifugation 12min, collect precipitation, precipitation priority distilled water and dehydrated alcohol are each washed 3 times, finally dry 3h in the electric drying oven with forced convection of 70 DEG C, can obtain Yb2SiO5Powder body.
Embodiment 3
A kind of Yb2SiO5Raw powder's production technology, comprises the following steps:
1) analytically pure Yb (NO) is weighed3·5H2O, is substantially soluble in dehydrated alcohol, is configured to the solution that concentration is 0.1mol/L, and the solution obtained is designated as solution A.
2) analytically pure tetraethyl orthosilicate (Si (OC is measured2H5)4), according to Yb (NO)3·5H2O: the mol ratio of tetraethyl orthosilicate=1:0.6, joins in solution A by the tetraethyl orthosilicate measured, and obtains solution B after being sufficiently stirred for 1h.
3) pouring in hydrothermal reaction kettle by solution B, be placed in constant temperature oven by reactor, controlling temperature is 90 DEG C, and the response time is 15h.
4) to be cooled after room temperature, take out and obtain wet gel, wet gel is put in thermostatic drier, controlling temperature is 70 DEG C, dry 7h, obtains powder body A.
5) dried powder body A is ground after put in crucible, be placed in Muffle furnace 400 DEG C of preheating 0.5h, after naturally cool to room temperature, after taking-up, obtain powder body B.
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O), by powder body B and Sodium Molybdate Dihydrate Homogeneous phase mixing, according to powder body B:Na2MoO4·2H2The mass ratio of O=1:1, is placed in Muffle furnace, controls temperature 800 DEG C, controls time 3h, obtains powder body C.By powder body C under 10000r/min, centrifugation 8min, collect precipitation, will precipitate, and successively each wash 5 times with distilled water and dehydrated alcohol, finally dry 3h in the electric drying oven with forced convection of 70 DEG C, can obtain Yb2SiO5Powder body.
Embodiment 4
A kind of Yb2SiO5Raw powder's production technology, comprises the following steps:
1) analytically pure Yb (NO) is weighed3·5H2O, is substantially soluble in dehydrated alcohol, is configured to the solution that concentration is 0.1mol/L, and the solution obtained is designated as solution A.
2) analytically pure tetraethyl orthosilicate (Si (OC is measured2H5)4), according to Yb (NO)3·5H2O: the mol ratio of tetraethyl orthosilicate=1:0.7, joins in solution A by the tetraethyl orthosilicate measured, and obtains solution B after being sufficiently stirred for 3h.
3) pouring in hydrothermal reaction kettle by solution B, be placed in constant temperature oven by reactor, controlling temperature is 100 DEG C, and the response time is 18h.
4) to be cooled after room temperature, take out and obtain wet gel, wet gel is put in thermostatic drier, controlling temperature is 80 DEG C, dry 8h, obtains powder body A.
5) dried powder body A is ground after put in crucible, be placed in Muffle furnace 400 DEG C of preheating 0.5h, after naturally cool to room temperature, after taking-up, obtain powder body B.
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O), by powder body B and Sodium Molybdate Dihydrate Homogeneous phase mixing, according to powder body B:Na2MoO4·2H2The mass ratio of O=1:1.5, is placed in Muffle furnace, controls temperature 750 DEG C, controls time 3h, obtains powder body C.By powder body C under 8000r/min, centrifugation 12min, collect precipitation, precipitation priority distilled water and dehydrated alcohol are each washed 5 times, finally dry 3h in the electric drying oven with forced convection of 80 DEG C, can obtain Yb2SiO5Powder body.
Embodiment 5
A kind of Yb2SiO5Raw powder's production technology, comprises the following steps:
1) analytically pure Yb (NO) is weighed3·5H2O, is substantially soluble in dehydrated alcohol, is configured to the solution that concentration is 0.1mol/L, and the solution obtained is designated as solution A.
2) analytically pure tetraethyl orthosilicate (Si (OC is measured2H5)4), according to Yb (NO)3·5H2O: the mol ratio of tetraethyl orthosilicate=1:0.8, joins in solution A by the tetraethyl orthosilicate measured, and obtains solution B after being sufficiently stirred for 1h.
3) pouring in hydrothermal reaction kettle by solution B, be placed in constant temperature oven by reactor, controlling temperature is 110 DEG C, and the response time is 24h.
4) to be cooled after room temperature, take out and obtain wet gel, wet gel is put in thermostatic drier, controlling temperature is 60 DEG C, dry 10h, obtains powder body A.
5) dried powder body A is ground after put in crucible, be placed in Muffle furnace 400 DEG C of preheating 1h, after naturally cool to room temperature, after taking-up, obtain powder body B.
6) commercially available analytically pure Sodium Molybdate Dihydrate (Na is selected2MoO4·2H2O), by powder body B and Sodium Molybdate Dihydrate Homogeneous phase mixing, according to powder body B:Na2MoO4·2H2The mass ratio of O=1:1, is placed in Muffle furnace, controls temperature 700 DEG C, controls time 3h, obtains powder body C.By powder body C under 9000r/min, centrifugation 10min, collect precipitation, precipitation priority distilled water and dehydrated alcohol are each washed 3 times, finally dry 3h in the electric drying oven with forced convection of 80 DEG C, can obtain Yb2SiO5Powder body.
Referring to Fig. 1, from FIG. 1, it can be seen that control temperature shown in XRD figure spectrum just can form ytterbium silicate (Yb at lower 700 DEG C2SiO5) crystalline phase, and diffraction maximum is obvious, keeps consistent with PDF card 40-0386.When fused salt, in liquid phase sodium molybdate, reacting substance mobility increases, and diffusion rate is significantly improved, and advantageously reduces the activation energy of reaction and the synthesis temperature of ytterbium silicate.
Referring to Fig. 2, same as above.When heat treatment temperature is 700 DEG C, ytterbium silicate (Yb2SiO5) powder crystallization is good, obtains the ytterbium silicate (Yb that size is comparatively homogeneous2SiO5) powder body, simultaneously because fused salt is applied between reactant powder body, prevent the reunion between granule, therefore in figure, powder reuniting is less, and powder body size is approximately 100～200nm.

Claims (10)

1. a Yb2SiO5Raw powder's production technology, it is characterised in that comprise the following steps:
1) Yb (NO) is taken3·5H2O, is dissolved in dehydrated alcohol, is configured to the solution A that concentration is 0.05～0.1mol/L；
2) by Yb (NO)3·5H2O: tetraethyl orthosilicate=1:(0.5～0.8) mol ratio, take Si (OC2H5)4, join in solution A, stir, obtained solution B；
3) solution B is carried out at 80～110 DEG C solvent thermal reaction, be subsequently cooled to room temperature, prepare wet gel, wet gel is dried, obtain powder body A；
4) by powder body A first pre-burning at 400 DEG C, it is cooled to room temperature, prepares powder body B；
5) by powder body B:Na2MoO4·2H2O=1:(1～2) mass ratio, by powder body B and Na2MoO4·2H2O is sufficiently mixed uniformly, sinters at 700～900 DEG C, prepares powder body C；
6), after powder body C being dissolved in water, be centrifuged separating, take precipitation, by after washing of precipitate, dry, prepare Yb2SiO5Powder body.
2. Yb according to claim 12SiO5Raw powder's production technology, it is characterised in that step 2) in, by Si (OC2H5)4Join and solution A is sufficiently stirred for 1～3h.
3. Yb according to claim 12SiO5Raw powder's production technology, it is characterised in that step 3) it is that solution B is placed in hydrothermal reaction kettle, reactor is placed in constant temperature oven and carries out solvent thermal reaction.
4. the Yb according to claim 1 or 32SiO5Raw powder's production technology, it is characterised in that the time of solvent thermal reaction is 12～24h.
5. Yb according to claim 12SiO5Raw powder's production technology, it is characterised in that step 3) it is that wet gel is placed in thermostatic drier, at 60～80 DEG C, dry 6～10h.
6. Yb according to claim 12SiO5Raw powder's production technology, it is characterised in that step 4) in, to put in crucible after powder body A is ground, then crucible is placed in Muffle furnace and carries out pre-burning, the preheating time is 0.5～1h.
7. Yb according to claim 12SiO5Raw powder's production technology, it is characterised in that step 5) in, by powder body B and Na2MoO4·2H2O is sufficiently mixed after uniformly, is placed in Muffle furnace and is sintered, and sintering time is 3～5h.
8. Yb according to claim 12SiO5Raw powder's production technology, it is characterised in that step 6) in, it is that precipitation is used distilled water, absolute ethanol washing 3～5 times successively.
9. Yb according to claim 12SiO5Raw powder's production technology, it is characterised in that step 6) described in centrifugal be when 8000～1000r/min, process 8～12min.
10. Yb according to claim 12SiO5Raw powder's production technology, it is characterised in that step 6) described in dry be dry 1～3h in the electric drying oven with forced convection of 60～80 DEG C.
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CN107759210A (en) * 2017-10-11 2018-03-06 中国航发北京航空材料研究院 A kind of Yb2SiO5The preparation method of spraying powder
CN110980748A (en) * 2019-12-31 2020-04-10 中南大学 Superfine ytterbium silicate powder material and preparation method and application thereof
CN111017982A (en) * 2019-12-31 2020-04-17 中南大学 Nano-grade rare earth silicate powder material and application thereof
CN116462507A (en) * 2023-04-13 2023-07-21 中山大学·深圳 Corrosion inhibitor and preparation method and application thereof

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CN103556224A (en) * 2013-11-04 2014-02-05 景德镇陶瓷学院 Method for preparing zirconium silicate whisker by employing non-hydrolytic sol-gel technology combined with molten-salt growth method

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