CN102605427A - Method for synthesizing tellurium barium molybdate (BaTeMo2O9) monocrystal micron powder - Google Patents

Method for synthesizing tellurium barium molybdate (BaTeMo2O9) monocrystal micron powder Download PDF

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CN102605427A
CN102605427A CN2012100942314A CN201210094231A CN102605427A CN 102605427 A CN102605427 A CN 102605427A CN 2012100942314 A CN2012100942314 A CN 2012100942314A CN 201210094231 A CN201210094231 A CN 201210094231A CN 102605427 A CN102605427 A CN 102605427A
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batemo
aluminate
powder
solid
barium
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CN102605427B (en
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李博
陶绪堂
陈丽丽
张中晗
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Shandong University
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Abstract

The invention discloses a method for synthesizing tellurium barium molybdate (BaTeMo2O9, BTM for short) monocrystal micron powder. According to the method, solid inorganic salt and solid oxides are used as raw materials, high-temperature and high-pressure water is used as reaction media, the BaTeMo2O9 monocrystal micron powder materials are synthesized in the condition ranges of 2 to 29MPa and 200 to 400 DEG C. The BaTeMo2O9 monocrystal micron powder materials synthesized by the method provided by the invention have the advantages that the phase is pure, the particle dimension range is 1 to 6 microns, and the dispersion performance is better. The invention provides a simple, convenient, safe and environment-friendly preparation process route for the synthesis of novel polybasic oxides.

Description

A kind of method of synthetic barium tellurium aluminate monocrystalline micron powder
Technical field
The present invention relates to a kind of preparation method of monocrystalline micrometer structure of oxide compound non-linear optic crystal, relate in particular to a kind of synthetic barium tellurium aluminate BaTeMo 2O 9The method of (being called for short BTM) monocrystalline micron powder, i.e. barium tellurium aluminate BaTeMo 2O 9The full solid phase raw material-HTHP hydrothermal system compound method of monocrystalline micron powder.
Background technology
Barium tellurium aluminate BaTeMo 2O 9Monocrystalline is a kind of novel non-linearity optical material.Relatively more rare to the research of this material at present, and compound method is very single.The barium tellurium aluminate bulk single crystal can be grown with flux method.Conventional solid state reaction can be used for synthesizing the barium tellurium aluminate polycrystal powder.But there are problems such as pattern inequality, serious agglomeration in conventional solid state reaction synthetic barium tellurium aluminate powder granule.Generally speaking, the granule-morphology of material is to its performance important influence, and particle size, shape variation all might cause the change on the performance.Particularly the powdered material particle size reaches the dimensional effect that is caused after the nanometer scale, always is the focus of attention in nano materials research field, has important scientific research meaning.
According to existing document, the supercritical water system has unique advantage aspect the special powder and micron powder material of synthetic this class formation of barium tellurium aluminate and performance.But the synthetic employed raw material of barium tellurium aluminate of the present supercritical water system of reporting is barium nitrate aqueous solution, tellurous oxide powder, molybdic oxide powder and potassium hydroxide aqueous solution.Barium nitrate aqueous solution and potassium hydroxide aqueous solution have been used in the above-mentioned reaction.Water-soluble barium ion toxicity is bigger, and Pottasium Hydroxide is a kind of highly basic, and therefore, experimentation has certain insecurity, also can cause problems such as environmental pollution.In addition, employed four kinds of reactant forms are different in the above-mentioned reaction, and might just react at mix stages between the reactant, finally influence the synthetic of barium tellurium aluminate, so this kind synthesis technique has strict demand to the addition sequence of raw material.When reactant according to potassium hydroxide aqueous solution, barium nitrate aqueous solution, tellurous oxide powder, could obtain the barium tellurium aluminate powder when this addition sequence of molybdic oxide powder mixes.So preparation of raw material process more complicated of present this synthetic process.
Summary of the invention
Deficiency and drawback to existing synthetic technology the invention provides a kind of simple and feasible synthetic barium tellurium aluminate BaTeMo 2O 9The method of (being called for short BTM) monocrystalline micron powder, i.e. barium tellurium aluminate BaTeMo 2O 9The full solid phase raw material-HTHP hydrothermal system compound method of monocrystalline micron powder.
Synthetic barium tellurium aluminate BaTeMo according to the invention 2O 9The method of monocrystalline micron powder, step is:
(1) batching: will be as synthetic target barium tellurium aluminate BaTeMo 2O 9In feed composition Ba, Te, Mo according to atomic ratio Ba: Te: Mo=1: 1: 2 ratio, mix with solid carbonic acid barium dust or solid oxidation barium dust, solid tellurous oxide powder and solid molybdic oxide form of powder;
(2) dispersed material: the mixed pressed powder of step (1) is scattered in the deionized water of its 40～100 times of volumes, forms the solid-liquid suspension body;
(3) isothermal reaction: the solid-liquid suspension body that step (2) obtains is put into the high-temperature high-voltage reaction container; After airtight reaction vessel put and be heated to 200～400 ℃ in the heating installation; Container inner pressure is 2～29MPa; Isothermal reaction 1～24 hour, this moment, the technical characterictic of reaction system was a HTHP hydro-thermal reaction system;
(4) cooling: after the isothermal reaction, reaction vessel is cooled to 20～25 ℃, container inner pressure is reduced to normal pressure;
(5) washing: adopt centrifugation or with the vacuum filtration device with solid in the reaction vessel and liquid separation, with deionized water, ethanol or washing with acetone gained solid precipitation at least 3 times, perhaps the liquid pH=7 after the washing ends;
(6) oven dry: the solid precipitation after step (5) washing is dried in 50～60 ℃ of conditions with drying plant, and the product of acquisition is the barium tellurium aluminate BaTeMo of pure phase 2O 9Monocrystalline micron powder.
Above-mentioned synthetic barium tellurium aluminate BaTeMo 2O 9In the method for monocrystalline micron powder: the said mixed pressed powder of step (2) preferably is scattered in the deionized water of its 40～70 times of volumes, forms the solid-liquid suspension body.
Above-mentioned synthetic barium tellurium aluminate BaTeMo 2O 9In the method for monocrystalline micron powder: preferably 300～400 ℃ of the said Heating temperatures of step (3), container inner pressure is preferably 10～29MPa, and the isothermal reaction time is preferably 1～8 hour.
Above-mentioned synthetic barium tellurium aluminate BaTeMo 2O 9In the method for monocrystalline micron powder: said high-temperature high-voltage reaction container is the high-temperature high-pressure reaction kettle that has thermometric, PMU.
Above-mentioned synthetic barium tellurium aluminate BaTeMo 2O 9In the method for monocrystalline micron powder: the said heating installation of step (3) is meant one of retort furnace, resistance furnace, tube furnace, baking oven of accurate controlled temperature device; Preferred retort furnace.
Above-mentioned synthetic barium tellurium aluminate BaTeMo 2O 9In the method for monocrystalline micron powder: the said refrigerative mode of step (4) is that well heater is cooled to room temperature according to setting speed; The stove internal cooling perhaps directly cuts off the power supply; Perhaps directly reaction vessel is taken out naturally cooling from well heater, be put in the frozen water after perhaps reaction vessel being taken out from well heater and cool off.
Above-mentioned synthetic barium tellurium aluminate BaTeMo 2O 9In the method for monocrystalline micron powder: the condition that the said centrifugation of step (5) is implemented is: 500～2000 rev/mins of centrifugal rotational speeds, centrifugation time 20～30 minutes.
Above-mentioned synthetic barium tellurium aluminate BaTeMo 2O 9In the method for monocrystalline micron powder: it is 0.2～0.5 micron that the said vacuum filtration device of step (5) adopts the aperture of filter filter membrane.
Above-mentioned synthetic barium tellurium aluminate BaTeMo 2O 9In the method for monocrystalline micron powder: the said drying plant of step (6) is baking oven, loft drier or infrared(ray)lamp.
Barium tellurium aluminate BaTeMo provided by the invention 2O 9The full solid phase raw material-HTHP hydrothermal system compound method of (being called for short BTM) monocrystalline powder and micron powder material can use safety, easy method to obtain barium tellurium aluminate BaTeMo 2O 9(being called for short BTM) monocrystalline micro-powder material has promoted the synthetic development that reaches sciemtifec and technical spheres such as application of novel non-linearity optical material.
Barium tellurium aluminate BaTeMo of the present invention 2O 9In the full solid phase raw material-HTHP hydrothermal system compound method of (being called for short BTM) monocrystalline powder and micron powder material; Solid phase inorganic salt and oxide compound by routine is raw material first; As reaction media, in 2～29MPa, 200～400 ℃ TR, synthesized barium tellurium aluminate BaTeMo with water 2O 9(being called for short BTM) monocrystalline powder and micron powder material.With this method synthetic barium tellurium aluminate BaTeMo 2O 9(being called for short BTM) monocrystalline powder and micron powder material, thing is mutually pure, and granule-morphology is more regular, and the difficult reunion of particle, and is dispersed relatively good.
The inventive method has been used the reactant feed of full solid phase; Use the HTHP hydrothermal system as reaction system; Greatly reduce toxicity and the pollution factor in the building-up process, simplified synthesis step, realized the control of building-up process and the control of product pattern easily.Because preparation of raw material, reaction process and conversion unit are fairly simple, the inventive method spy is suitable for industrialized mass production.
Barium tellurium aluminate BaTeMo provided by the invention 2O 9All solid state raw material-HTHP hydrothermal system the compound method of (being called for short BTM) monocrystalline powder and micron powder material also is applicable to the synthetic of some composite oxide single crystal micro materials, is a kind of universal method of synthesizing oxygen-containing inorganic metal compound.
Description of drawings
Fig. 1: the BaTeMo that adopts full solid phase raw material-HTHP hydrothermal system compound method preparation 2O 9Crystallite.
Wherein: Fig. 1 a is an X-ray diffracting spectrum; Fig. 1 b is a stereoscan photograph.
Fig. 2: the BaTeMo that adopts full solid phase raw material-HTHP hydrothermal system compound method preparation 2O 9Crystallite.
Wherein: Fig. 2 a is an X-ray diffracting spectrum; Fig. 2 b is a stereoscan photograph.
Fig. 3: the BaTeMo that adopts full solid phase raw material-HTHP hydrothermal system compound method preparation 2O 9Crystallite.
Wherein: Fig. 3 a is an X-ray diffracting spectrum; Fig. 3 b is a stereoscan photograph.
Fig. 4: the BaTeMo that adopts full solid phase raw material-HTHP hydrothermal system compound method preparation 2O 9Crystallite.
Wherein: Fig. 4 a is an X-ray diffracting spectrum; Fig. 4 b is a stereoscan photograph.
Fig. 5: the BaTeMo that adopts full solid phase raw material-HTHP hydrothermal system compound method preparation 2O 9Crystallite.
Wherein: Fig. 5 a is an X-ray diffracting spectrum; Fig. 5 b is a stereoscan photograph.
Fig. 6: the BaTeMo that adopts full solid phase raw material-HTHP hydrothermal system compound method preparation 2O 9Crystallite.
Wherein: Fig. 6 a is an X-ray diffracting spectrum; Fig. 6 b is a stereoscan photograph.
Embodiment
Embodiment 1
1. prepare burden:
0.2960 gram barium carbonate, 0.2394 gram tellurous oxide and 0.4319 gram molybdic oxide are distributed in 50 ml deionized water.Join in the high-temperature high-pressure reaction kettle (volume is 100 milliliters) that has thermometric, PMU sealing then.
2. isothermal reaction:
The reaction kettle of sealing is put into retort furnace, and (container inner pressure reaches 22～25MPa), under this temperature constant 1 hour to be heated to 380 ℃.
3. cooling:
Make reaction kettle naturally cool to room temperature (20 ℃～25 ℃), reaction kettle is taken out from retort furnace.
4. washing:
From reaction kettle, take out product, product is filtered through vacuum filter (aperture is 0.45 micron), obtain solid sediment; The liquid pH=7 that arrives after the washing with deionized water, washing with alcohol gained solid precipitation ends.
5. oven dry:
With drying in the baking oven of solid under 50 ℃～60 ℃ temperature that obtains after filtering, obtain BaTeMo 2O 9Powder.
X-ray diffraction is the result show, the powder that experiment obtains is monocline phase barium tellurium aluminate BaTeMo 2O 9(Fig. 1 a).Sem observation shows that powder is the polyhedron particle (Fig. 1 b) of 1～2 micron of mean sizes.
Embodiment 2
1. prepare burden:
0.2960 gram barium carbonate, 0.2394 gram tellurous oxide and 0.4319 gram molybdic oxide are distributed in 50 ml deionized water.Join in the high-temperature high-pressure reaction kettle (volume is 100 milliliters) that has thermometric, PMU sealing then.
2. isothermal reaction:
The reaction kettle of sealing is put into retort furnace, and (container inner pressure reaches 26～29MPa), under this temperature constant 2 hours to be heated to 400 ℃.
3. cooling:
Make reaction kettle naturally cool to room temperature (20 ℃～25 ℃), reaction kettle is taken out from retort furnace.
4. washing:
From reaction kettle, take out product, product is filtered through vacuum filter (aperture is 0.45 micron), obtain solid sediment; With deionized water, washing with acetone gained solid precipitation 6 times;
5. oven dry:
With drying in the loft drier of solid under 50 ℃～60 ℃ temperature that obtains after filtering, obtain BaTeMo 2O 9Powder.
X-ray diffraction is the result show, the powder that experiment obtains is monocline phase barium tellurium aluminate BaTeMo 2O 9(Fig. 2 a).Sem observation shows that powder is the polyhedron particle (Fig. 2 b) of 4～5 microns of mean sizess.
Embodiment 3
1. prepare burden:
0.2960 gram barium carbonate, 0.2394 gram tellurous oxide and 0.4319 gram molybdic oxide are distributed in 50 ml deionized water.Join in the high-temperature high-pressure reaction kettle (volume is 100 milliliters) that has thermometric, PMU sealing then.
2. isothermal reaction:
The reaction kettle of sealing is put into resistance furnace, and (container inner pressure reaches 22～25MPa), under this temperature constant 4 hours to be heated to 380 ℃.
3. cooling:
Be put into after reaction kettle taken out from resistance furnace and be cooled to room temperature (20 ℃～25 ℃) in the frozen water.
4. washing:
From reaction kettle, take out product, product is filtered through vacuum filter (aperture is 0.22 micron), obtain solid sediment; With deionized water, washing with alcohol gained solid precipitation 5 times.
5. oven dry:
The solid that obtains after filtering under infrared(ray)lamp, with 50 ℃～60 ℃ temperature condition oven dry, is obtained BaTeMo 2O 9Powder.
X-ray diffraction is the result show, the powder that experiment obtains is monocline phase barium tellurium aluminate BaTeMo 2O 9(Fig. 3 a).Sem observation shows that powder is the polyhedron particle (Fig. 3 b) of 2 microns of mean sizess.
Embodiment 4
1. prepare burden:
0.2960 gram barium carbonate, 0.2394 gram tellurous oxide and 0.4319 gram molybdic oxide are distributed in 50 ml deionized water.Join in the high-temperature high-pressure reaction kettle (volume is 100 milliliters) that has thermometric, PMU sealing then.
2. isothermal reaction:
The reaction kettle of sealing is put into tube furnace, and (container inner pressure reaches 7～10MPa), under this temperature constant 8 hours to be heated to 300 ℃.
3. cooling:
Make reaction kettle naturally cool to room temperature (20 ℃～25 ℃), reaction kettle is taken out from tube furnace.
4. washing:
From reaction kettle, take out product,, centrifugal 30 minutes, obtain solid sediment with 1000 rev/mins of rotating speeds; With deionized water, washing with acetone gained solid precipitation 8 times;
5. oven dry:
The solid that obtains after filtering is dried under 50 ℃～60 ℃ temperature, obtain BaTeMo 2O 9Powder.
X-ray diffraction is the result show, the powder that experiment obtains is monocline phase barium tellurium aluminate BaTeMo 2O 9(Fig. 4 a).Sem observation shows that most powder particles are writing board shape, 4～5 microns of size ranges.Few granules pattern irregularity (Fig. 4 b).
Embodiment 5
1. prepare burden:
0.2300 gram barium oxide, 0.2394 gram tellurous oxide and 0.4319 gram molybdic oxide are distributed in 50 ml deionized water.Join in the high-temperature high-pressure reaction kettle (volume is 100 milliliters) that has thermometric, PMU sealing then.
2. isothermal reaction:
The reaction kettle of sealing is put into retort furnace, and (container inner pressure reaches 22～25MPa), under this temperature constant 2 hours to be heated to 380 ℃.
3. cooling:
Make reaction kettle naturally cool to room temperature (20 ℃～25 ℃), reaction kettle is taken out from retort furnace.
4. washing:
From reaction kettle, take out product,, centrifugal 20 minutes, obtain solid sediment with 1500 rev/mins of rotating speeds; The liquid pH=7 that arrives after the washing with deionized water, washing with alcohol gained solid precipitation ends.
5. oven dry:
The solid that obtains after filtering is dried under 50 ℃～60 ℃ temperature, obtain BaTeMo 2O 9Powder.
X-ray diffraction is the result show, the powder that experiment obtains is monocline phase barium tellurium aluminate BaTeMo 2O 9(Fig. 5 a).Sem observation shows that powder is the polyhedron particle (Fig. 5 b) of 1 micron of mean sizes.
Embodiment 6
1. prepare burden:
0.2960 gram barium carbonate, 0.2394 gram tellurous oxide and 0.4319 gram molybdic oxide are distributed in 50 ml deionized water.Join in the high-temperature high-pressure reaction kettle (volume is 100 milliliters) that has thermometric, PMU sealing then.
2. isothermal reaction:
The reaction kettle of sealing is put into baking oven, be heated to 200 ℃ (container inner pressure 2MPa), under this temperature constant 24 hours.
3. cooling:
Make reaction kettle naturally cool to room temperature (20 ℃～25 ℃), reaction kettle is taken out from baking oven.
4. washing:
From reaction kettle, take out product, product is filtered through vacuum filter (aperture is 0.22 micron), obtain solid sediment; The liquid pH=7 that arrives after the washing with deionized water, washing with acetone gained solid precipitation ends.
5. oven dry:
The solid that obtains after filtering is dried under 50 ℃～60 ℃ temperature, obtain BaTeMo 2O 9Powder.
X-ray diffraction is the result show, the powder that experiment obtains is monocline phase barium tellurium aluminate BaTeMo 2O 9(Fig. 6 a).Sem observation shows that powder particle is irregular writing board shape, 4～6 microns of size ranges.Part granule-morphology irregularity (Fig. 6 b) is arranged.

Claims (9)

1. synthetic barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder, step is:
(1) batching: will be as synthetic target barium tellurium aluminate BaTeMo 2O 9In feed composition Ba, Te, Mo according to atomic ratio Ba: Te: Mo=1: 1: 2 ratio, mix with solid carbonic acid barium dust or solid oxidation barium dust, solid tellurous oxide powder and solid molybdic oxide form of powder;
(2) dispersed material: the mixed pressed powder of step (1) is scattered in the deionized water of its 40～100 times of volumes, forms the solid-liquid suspension body;
(3) isothermal reaction: the solid-liquid suspension body that step (2) obtains is put into the high-temperature high-voltage reaction container; After airtight reaction vessel put and be heated to 200～400 ℃ in the heating installation; Container inner pressure is 2～29MPa; Isothermal reaction 1～24 hour, this moment, the technical characterictic of reaction system was a HTHP hydro-thermal reaction system;
(4) cooling: after the isothermal reaction, reaction vessel is cooled to 20～25 ℃, container inner pressure is reduced to normal pressure;
(5) washing: adopt centrifugation or with the vacuum filtration device with solid in the reaction vessel and liquid separation, with deionized water, ethanol or washing with acetone gained solid precipitation at least 3 times, perhaps the liquid pH=7 after the washing ends;
(6) oven dry: the solid precipitation after step (5) washing is dried in 50～60 ℃ of conditions with drying plant, and the product of acquisition is the barium tellurium aluminate BaTeMo of pure phase 2O 9Monocrystalline micron powder.
2. synthetic according to claim 1 barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder is characterized in that: the said mixed pressed powder of step (2) is scattered in the deionized water of its 40～70 times of volumes, forms the solid-liquid suspension body.
3. synthetic according to claim 1 barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder is characterized in that: the said Heating temperature of step (3) is 300～400 ℃, and container inner pressure is 10～29MPa, and the isothermal reaction time is 1～8 hour.
4. synthetic according to claim 1 barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder is characterized in that: the said high-temperature high-voltage reaction container of step (3) is the high-temperature high-pressure reaction kettle that has thermometric, PMU.
5. synthetic according to claim 1 barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder is characterized in that: the said heating installation of step (3) is meant one of retort furnace, resistance furnace, tube furnace, baking oven of accurate controlled temperature device.
6. synthetic according to claim 1 barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder; It is characterized in that: the said refrigerative mode of step (4) is that well heater is cooled to room temperature according to setting speed; The stove internal cooling perhaps directly cuts off the power supply; Perhaps directly reaction vessel is taken out naturally cooling from well heater, be put in the frozen water after perhaps reaction vessel being taken out from well heater and cool off.
7. synthetic according to claim 1 barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder is characterized in that: the condition that the said centrifugation of step (5) is implemented is: 500～2000 rev/mins of centrifugal rotational speeds, centrifugation time 20～30 minutes.
8. synthetic according to claim 1 barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder is characterized in that: it is 0.2～0.5 micron that the said vacuum filtration device of step (5) adopts the aperture of filter filter membrane.
9. synthetic according to claim 1 barium tellurium aluminate BaTeMo 2O 9The method of monocrystalline micron powder is characterized in that: the said drying plant of step (6) is baking oven, loft drier or infrared(ray)lamp.
CN201210094231.4A 2012-04-01 2012-04-01 Method for synthesizing tellurium barium molybdate (BaTeMo2O9) monocrystal micron powder Expired - Fee Related CN102605427B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103031592A (en) * 2013-01-21 2013-04-10 山东大学 Method for synthesizing tellurium molybdate magnesium single crystal micro powder by using supercritical water system
CN107841786A (en) * 2017-10-31 2018-03-27 中国科学院福建物质结构研究所 A kind of inorganic compound crystal, its preparation method and application

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Publication number Priority date Publication date Assignee Title
CN102031563A (en) * 2010-09-30 2011-04-27 山东大学 High-temperature-phase tellurium barium molybdate crystal as well as preparation method and applications thereof

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Publication number Priority date Publication date Assignee Title
CN102031563A (en) * 2010-09-30 2011-04-27 山东大学 High-temperature-phase tellurium barium molybdate crystal as well as preparation method and applications thereof

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WILLIAM T. A. HARRISON ET AL: "Hydrothermal Investigation of the Barium/Molybdenum(VI)/Selenium(IV) Phase Space: Single-Crystal Structures of BaMoO3SeO3 and BaMo2O5(SeO3)2", 《JOURNAL OF SOLID STATE CHEMISTRY》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103031592A (en) * 2013-01-21 2013-04-10 山东大学 Method for synthesizing tellurium molybdate magnesium single crystal micro powder by using supercritical water system
CN107841786A (en) * 2017-10-31 2018-03-27 中国科学院福建物质结构研究所 A kind of inorganic compound crystal, its preparation method and application
CN107841786B (en) * 2017-10-31 2019-10-29 中国科学院福建物质结构研究所 A kind of inorganic compound crystal, preparation method and application

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