CN107382315A - A kind of lanthanum molybdate sodium nano material and preparation method thereof - Google Patents

A kind of lanthanum molybdate sodium nano material and preparation method thereof Download PDF

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CN107382315A
CN107382315A CN201710524958.4A CN201710524958A CN107382315A CN 107382315 A CN107382315 A CN 107382315A CN 201710524958 A CN201710524958 A CN 201710524958A CN 107382315 A CN107382315 A CN 107382315A
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lanthanum
nano material
molybdate
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mixed
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CN107382315B (en
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林志东
罗京
付萍
陈喆
邓泉荣
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Wuhan Institute of Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract

The present invention relates to a kind of lanthanum molybdate sodium nano material and preparation method thereof, the lanthanum molybdate sodium nano material purity is more than 99%, and average grain size is 20 100nm.Its preparation methods steps are：1) lanthanum nitrate hexahydrate, sodium molybdate are dissolved in the mixed solvent respectively, obtain solution containing lanthanum and containing molybdenum solution；2) solution containing lanthanum obtained by step 1) is mixed with containing molybdenum solution, then mixed liquor is placed in hydrothermal reaction kettle and carries out solvent thermal reaction, reaction is filtered after terminating, washs, is dried to obtain lanthanum molybdate sodium nano material.Lanthanum molybdate sodium nano material prepared by the present invention is applied to LTCC field, can be used as the base-material of ltcc substrate, encapsulating material, and higher with dielectric constant, co-fired temperature is low, the advantages that not reacted with Ag.

Description

A kind of lanthanum molybdate sodium nano material and preparation method thereof
Technical field
The invention belongs to microwave-medium ceramics technical field, and in particular to a kind of lanthanum molybdate sodium nano material and its preparation side Method.
Background technology
LTCC (Low-temperature cofired ceramics, LTCC) technology, exactly burns low temperature The accurate and fine and close green band of thickness is made in knot ceramic powder, as circuit base material, on green band using laser boring, The techniques such as micropore slip casting, the printing of accurate conductor paste make required circuitous pattern, and by the embedment of multiple passive elements wherein, Then overlap together, in 900 DEG C of sintering, the passive integration component of three-dimensional circuit network is made, may be made as built-in passive member The three-dimensional circuit substrate of part, IC and active device can be mounted on its surface, passive/active integrated functional module is made, is One kind is used to realize high integration, high performance Electronic Encapsulating Technology.
But sintering temperature to be present too high (higher than common metal Ag, Cu etc. fusing point) for conventional microwave dielectric ceramic materials The problem of, it is impossible to burnt altogether with metal, it is difficult to applied in LTCC Technology.To adapt to microwave electron component in microwave The requirement developed in circuit to miniaturization, integrated, inexpensive direction, exploitation low temperature co-fired microwave dielectric ceramics are necessary 's.
The dielectric constant of lanthanum molybdate sodium ceramics is less than the fusing point of common metal, it is micro- to can be used as low temperature in 10-13, sintering temperature Ripple media ceramic is used for a variety of electronic components, such as resonator, wave filter.But the synthesis of current lanthanum molybdate sodium is mostly using solid After phase synthesi, or liquid-phase precipitation prepared by the method for sintering processes, and its preparation process reaction temperature is high, and product purity is low, energy Consumption is high.Exploitation synthesis high-purity, the lanthanum molybdate sodium ceramic material with low-temperature sintering performance have great importance.
The content of the invention
The technical problems to be solved by the invention are for above shortcomings in the prior art, there is provided a kind of high-purity Lanthanum molybdate sodium nano material and preparation method thereof.
In order to solve the above technical problems, technical scheme provided by the invention is：
A kind of lanthanum molybdate sodium nano material is provided, the lanthanum molybdate sodium nano material purity is more than 99%, average crystal grain Size is 20-100nm.
The present invention also provides the preparation method of above-mentioned lanthanum molybdate sodium nano material, and its step is as follows：
1) lanthanum nitrate hexahydrate, sodium molybdate are dissolved in the mixed solvent respectively, the mixed solvent by ethylene glycol or glycerine with Water 1-2: 1 is mixed to get by volume, obtains solution containing lanthanum and containing molybdenum solution；
2) solution containing lanthanum obtained by step 1) is mixed with containing molybdenum solution, obtains mixed liquor so that lanthanum, molybdenum element in mixed liquor Mol ratio is 0.8-1.2: 2, and then mixed liquor is placed in hydrothermal reaction kettle and carries out solvent thermal reaction, reaction terminate after filtering, Wash, be dried to obtain lanthanum molybdate sodium nano material.
By such scheme, the mass concentration of lanthanum nitrate hexahydrate is 1-15% in solution containing lanthanum described in step 1)；It is described to contain molybdenum The mass concentration of Molybdenum in Solution acid sodium is 1-15%.
By such scheme, the condition of the step 2) solvent thermal reaction is：1-12h is reacted at 120-200 DEG C.
Preferably, the solution compactedness of the step 2) hydrothermal reaction kettle is 60-80%.
Present invention additionally comprises application of the above-mentioned lanthanum molybdate sodium nano material in terms of low temperature co-fired microwave dielectric ceramics.
The beneficial effects of the present invention are：The present invention is using glycol/water or glycerin/water as mixed solvent, lanthanum nitrate hexahydrate It is that raw material carries out lanthanum molybdate sodium nano material of the solvent thermal reaction through single step reaction preparation high-purity, nontoxic solvent ring with sodium molybdate Protect, technique is simple, and reaction condition is gentle, and the lanthanum molybdate sodium nano material has the higher (dielectric constant=10- of dielectric constant 13), dielectric loss low (Qf about 25050GHz), temperature coefficient of resonance frequency low (TCF=-40--48ppm/ DEG C), co-fired temperature Low (about 700 DEG C), and the advantages that do not reacted with Ag, suitable for low temperature microwave medium ceramic field, can be used as LTCC bases Plate, encapsulating material base-material and prepare a variety of electronic components, such as resonator, wave filter.
Brief description of the drawings
Fig. 1 is the XRD piece of the lanthanum molybdate sodium nano material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM pictures of the lanthanum molybdate sodium nano material prepared by embodiment 1.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made below in conjunction with the accompanying drawings into One step is described in detail.
Embodiment 1
Nanometer lanthanum molybdate sodium is prepared, step is as follows：
1) by 585g (1mol) La (NO3)3·6H2The in the mixed solvent of 2L glycerine and 2L water is dissolved under O stirrings, is contained Lanthanum solution, then by 484g (2mol) Na2MoO4·2H2The in the mixed solvent of another 2L glycerine and 2L water is dissolved under O stirrings, is obtained To containing molybdenum solution；
2) lanthanum solution will be contained to mix with containing molybdenum solution, gained mixed liquor is transferred to (reactor in sealing 10L autoclaves Solution compactedness 80%), be warming up to 200 DEG C and react 1 hour, reactor is then naturally cooled into room temperature, products therefrom warp Centrifugal filtration, deionized water washing, gained powder is dried 2 hours at 150 DEG C, obtains lanthanum molybdate sodium ceramic powder.
The present embodiment products therefrom is subjected to X-ray diffraction analysis, XRD is as shown in Figure 1, it is known that product is lanthanum molybdate sodium Material, purity are more than 99%, and product SEM figures are shown in Fig. 2, and lanthanum molybdate sodium material average grain diameter is 50nm as seen from the figure, dielectric constant For 11.3, dielectric loss 25050GHz, temperature coefficient of resonance frequency is low (TCF=-46ppm/ DEG C), and sintering temperature is 700 DEG C.
Embodiment 2
Nanometer lanthanum molybdate sodium is prepared, step is as follows：
1) by 468g (0.8mol) La (NO3)3·6H2The in the mixed solvent of 2L ethylene glycol and 2L water is dissolved under O stirrings, is obtained To solution containing lanthanum, then by 484g (2mol) Na2MoO4·2H2The mixed solvent of another 2L ethylene glycol and 2L water is dissolved under O stirrings In, obtain containing molybdenum solution；
2) lanthanum solution will be contained to mix with containing molybdenum solution, gained mixed liquor is transferred to (reactor in sealing 10L autoclaves Solution compactedness 80%), be warming up to 120 DEG C and react 12 hours, reactor is then naturally cooled into room temperature, products therefrom warp Centrifugal filtration, deionized water washing, gained powder is dried 12 hours at 60 DEG C, obtains lanthanum molybdate sodium ceramic powder.
The present embodiment products therefrom is tested, it is known that product is lanthanum molybdate sodium nano material, and purity is more than 99%, puts down Equal particle diameter is 30nm, dielectric constant 11.0, dielectric loss 25050GHz, the low (TCF=-48ppm/ of temperature coefficient of resonance frequency DEG C), sintering temperature is 700 DEG C.
Embodiment 3
Nanometer lanthanum molybdate sodium is prepared, step is as follows：
1) by 70.2g (0.12mol) La (NO3)3·6H2The mixing that 500mL ethylene glycol and 500mL water are dissolved under O stirrings is molten In agent, solution containing lanthanum is obtained, then by 48.4g (0.2mol) Na2MoO4·2H2O stirring under be dissolved in another 250mL ethylene glycol with The in the mixed solvent of 250mL water, obtain containing molybdenum solution；
2) lanthanum solution will be contained to mix with containing molybdenum solution, gained mixed liquor is transferred to (reactor in sealing 2L autoclaves Solution compactedness 75%), be warming up to 160 DEG C and react 6 hours, reactor is then naturally cooled into room temperature, products therefrom warp Centrifugal filtration, deionized water washing, gained powder is dried 10 hours at 80 DEG C, obtains lanthanum molybdate sodium ceramic powder.
The present embodiment products therefrom is tested, it is known that product is lanthanum molybdate sodium nano material, and purity is more than 99%, puts down Equal particle diameter is 40nm, dielectric constant 13.0, dielectric loss 25050GHz, the low (TCF=-48ppm/ of temperature coefficient of resonance frequency DEG C), sintering temperature is 700 DEG C.
Embodiment 4
Nanometer lanthanum molybdate sodium is prepared, step is as follows：
1) by 58.5g (0.1mol) La (NO3)3·6H2The mixing that 600mL ethylene glycol and 300mL water are dissolved under O stirrings is molten In agent, solution containing lanthanum is obtained, then by 48.4g (0.2mol) Na2MoO4·2H2O stirring under be dissolved in another 300mL ethylene glycol with The in the mixed solvent of 150mL water, obtain containing molybdenum solution；
2) lanthanum solution will be contained to mix with containing molybdenum solution, gained mixed liquor is transferred to (reactor in sealing 2L autoclaves Solution compactedness 68%), be warming up to 180 DEG C and react 6 hours, reactor is then naturally cooled into room temperature, products therefrom warp Centrifugal filtration, deionized water washing, gained powder is dried 10 hours at 80 DEG C, obtains lanthanum molybdate sodium ceramic powder.
The present embodiment products therefrom is tested, it is known that product is lanthanum molybdate sodium nano material, and purity is more than 99%, puts down Equal particle diameter is 40nm, dielectric constant 13.0, dielectric loss 25050GHz, the low (TCF=-48ppm/ of temperature coefficient of resonance frequency DEG C), sintering temperature is 700 DEG C.
It the foregoing is only the preferred embodiment of the present invention, it is noted that come for one of ordinary skill in the art Say, without departing from the concept of the premise of the invention, make some modifications and variations, these belong to the protection model of the present invention Enclose.

Claims (5)

  1. A kind of 1. lanthanum molybdate sodium nano material, it is characterised in that：The lanthanum molybdate sodium nano material purity is more than 99%, average Crystallite dimension is 20-100nm.
  2. 2. the preparation method of the lanthanum molybdate sodium nano material described in a kind of claim 1, it is characterised in that step is as follows：
    1) lanthanum nitrate hexahydrate, sodium molybdate are dissolved in the mixed solvent respectively, the mixed solvent is pressed by ethylene glycol or glycerine with water Volume ratio 1-2:1 is mixed to get, and obtains solution containing lanthanum and containing molybdenum solution；
    2) solution containing lanthanum obtained by step 1) is mixed with containing molybdenum solution, obtains mixed liquor so that lanthanum, molybdenum element mole in mixed liquor Than for 0.8-1.2：2, then mixed liquor is placed in hydrothermal reaction kettle and carries out solvent thermal reaction, reaction terminate after filtering, washing, It is dried to obtain lanthanum molybdate sodium nano material.
  3. 3. preparation method according to claim 2, it is characterised in that lanthanum nitrate hexahydrate in solution containing lanthanum described in step 1) Mass concentration is 1-15%；The mass concentration containing sodium molybdate in molybdenum solution is 1-15%.
  4. 4. preparation method according to claim 2, it is characterised in that the condition of the step 2) solvent thermal reaction is：In 1-12h is reacted at 120-200 DEG C.
  5. 5. application of the lanthanum molybdate sodium nano material according to claim 1 in terms of low temperature co-fired microwave dielectric ceramics.
CN201710524958.4A 2017-06-30 2017-06-30 Sodium lanthanum molybdate nano material and preparation method thereof Active CN107382315B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108190957A (en) * 2018-03-18 2018-06-22 中船重工黄冈贵金属有限公司 A kind of preparation method of flower-shaped cerous molybdate sodium nanometer rods cluster

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108190957A (en) * 2018-03-18 2018-06-22 中船重工黄冈贵金属有限公司 A kind of preparation method of flower-shaped cerous molybdate sodium nanometer rods cluster

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