CN106747428A - The preparation method of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder - Google Patents
The preparation method of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder Download PDFInfo
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- CN106747428A CN106747428A CN201710027468.3A CN201710027468A CN106747428A CN 106747428 A CN106747428 A CN 106747428A CN 201710027468 A CN201710027468 A CN 201710027468A CN 106747428 A CN106747428 A CN 106747428A
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Abstract
It is 1 according to Hf and Y mol ratios with yttrium nitrate and hafnium tetrachloride or oxychlorination hafnium as raw material the present invention relates to a kind of preparation method of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder:1 metering is than configuration precursor solution, selection glucose, glycine, citric acid, ethylenediamine tetra-acetic acid and urea etc. are used as incendiary agent, optimum organization, regulation solution ph is in the range of 1~6, solution is placed in and is warmed up in 250~800 DEG C of Muffle furnace in advance, solvent combustion synthesis puffy material, 1~4h is heat-treated at 350~800 DEG C, and one-step method obtains crystallite dimension in 5~200nm hafniums acid yttrium nanocrystalline powder., compared to solid phase method and coprecipitation method, synthesis temperature is relatively low, and the time cycle is shorter, even grain size for this method, the features such as being produced on a large scale.
Description
Technical field
The invention belongs to powder synthesis field, it is related to a kind of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder
Preparation method.
Background technology
Hafnium acid yttrium (Y2Hf2O7) at normal temperatures in cube pyrochlore constitution of stabilization, possess high density, effective atomic mumber high
The good characteristics such as ray absorption capacity several, high, so hafnium acid yttrium material is at aspects such as information detection, laser medium, high-temperature windows
There is good application prospect.The yttrium of hafnium acid simultaneously also has high temperature stability performance, thermal coefficient of expansion high and low thermal conductivity, is one
Plant new barrier material.
When in the microstructure of ceramic material, crystal grain, crystal boundary and the combination between them are at claiming during nano-scale
It is nano ceramics.Due to the refinement of nano ceramics crystal grain, the increase of crystal boundary number can obtain intensity, toughness and the superplasticity of material
To very big raising, and the performance such as electricity, calorifics, magnetics, optics to material produces important influence.
The method of the preparation of nanocrystalline ceramics powder has various, and soft chemical classes method has coprecipitation, sol-gal process, molten
Agent thermal synthesis method, microwave-hydrothermal method and combustion method etc..Nanocrystalline powder prepared by the present invention uses combustion synthesis, combustion method
Fast relative to other several method aggregate velocities, synthesis temperature is low beneficial to large-scale production.
Yetta Eagleman of Lao Lunsi Berkeleys National Key Laboratory etc. use La2O3And HfO21400~1600
DEG C Solid phase synthesis La2Hf2O7.The Zeming Qi La of Chinese University of Science and Technology2O3And HfO2Solid state reaction kinetics
La2Hf2O7Have studied its molecular vibration and dielectric properties.Belgrade universityJelena Papan HfCl4And yittrium oxide
It is former material, material polyethylene glycol (PEG) obtains colloidal sol for chelating agent at 120 DEG C, then obtains average crystalline substance under different temperatures roasting
Particle size is the Y of 3~500nm yardsticks2Hf2O7Powder.The Yikun Liao of Shanghai silicate research institute are with Y (NO3)3And HfO
(NO3)2For the mixed liquor of raw material glycine, urea or glycine and urea is incendiary agent, EDTA is chelating agent, obtained
Y2Hf2O7Powder is in the range of 30~300nm.The Karl R.Whittle of Australia at 1500 DEG C of solid phase method having synthesized one
The La of series2-xYxZr2O7And La2-xYxHf2O7Ceramics grind and have studied carefully its structure and chemical feature.The Linggen of Australia
Kong softening methods have synthesized Y2HfxTi2-xO7, he uses HfCl4, Tyzor LA and yttrium nitrate be raw material, glucose is for also
Former agent obtains Y in 80 DEG C of drying and then 700 DEG C of roastings2HfxTi2-xO7The ceramic powder of component.Shanghai silicate research institute
Guohong Zhou are with (Y (NO3)3·6H2O and HfO2It is presoma, ball milling 12h under alcoholic environment is then calcined at 800 DEG C
2h obtains precursor powder, and vacuum-sintering obtains Y at 1900 DEG C2Hf2O7Crystalline ceramics.The Zou little Qing of Shanghai silicate research institute
Deng with yttrium nitrate (Y (NO3)3) and hafnium chloride (HfCl4) be raw material, ethylenediamine tetra-acetic acid (EDTA) as incendiary agent, using burning
It is the pure phase hafnium acid yttrium powder body of 50nm or so that method is prepared for particle diameter.The Zhou Guohong of Shanghai silicate research institute is with yttrium nitrate, tetrachloro
It is that raw material is prepared for 150~250nm of grain size nanometers of hafnium acid yttrium powder body using coprecipitation to change hafnium and ammonium oxalate.
The content of the invention
The technical problem to be solved
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of one-step synthesis method various grain sizes hafnium acid yttrium
The preparation method of ceramic powder, precursor solution is configured with yttrium nitrate and hafnium tetrachloride or oxychlorination hafnium as raw material, and selection is suitable
Incendiary agent, under certain heat treating regime, the hafnium acid yttrium ceramic powder of various grain sizes is obtained.
Technical scheme
A kind of preparation method of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder, it is characterised in that step is such as
Under：
The preparation of step 1, presoma：By hafnium tetrachloride HfCl4Or oxychlorination hafnium is dissolved in deionized water, excess is added
Ammoniacal liquor, obtains without Cl-The sediment of ion；It is placed in again in magnetic agitation water-bath, adds excessive nitric acid, dissolution precipitation thing
Until presented in beaker being free of Cl-The transparency liquid of ion；
Step 2：It is 1 according to Hf and Y mol ratios:1 metering obtains yttrium nitrate addition step 1 than weighing yttrium nitrate
Transparency liquid in form mixed solution；
Carbon containing or nitrogenous incendiary agent is added to mixed solution, while adding ammoniacal liquor and nitric acid, regulation solution ph is 1
~6；The calculating of the incendiary agent carries out dispensing using the flat perseverance principle of chemical valence according to 0.6~1.6 times of the incendiary agent for being calculated
Calculate；
Step 3：The beaker of mixed solution will be filled, is placed in and is raised in the Muffle furnace that temperature is 200~800 DEG C in advance, with
The volatilization of solvent, solution concentration constantly increases, and collosol and gel is gradually formed, last solution combustion obtains puffy material；
Step 4：It it is 350~800 DEG C in temperature by the heat treatment of puffy material, heat treatment time is 1~4h, is removed many
Remaining carbon residue obtains the hafnium acid yttrium white powder of various grain sizes.
The step 1 is changed to：Hafnium tetrachloride or oxychlorination hafnium are directly substantially soluble in deionized water, are sufficiently stirred for being formed
Containing Cl-The transparency liquid of ion；Then the hafnium acid yttrium white powder that step 2~step 4. obtains various grain sizes is carried out.
The incendiary agent is pure for analysis, including：Urea, citric acid, edta edta, glucose, ethanol or sweet
The combination of one or more incendiary agents in propylhomoserin.
The hafnium tetrachloride HfCl4With oxychlorination hafnium HfCl2O·8H2It is pure that O is analysis.
Yttrium nitrate Y (the NO3)3·6H2O is pure or high-purity for analysis.
Beneficial effect
The preparation method of a kind of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder proposed by the present invention, with nitric acid
Yttrium and hafnium tetrachloride or oxychlorination hafnium are raw material, are 1 according to Hf and Y mol ratios:1 metering is than configuration precursor solution, selection
Glucose, glycine, citric acid, ethylenediamine tetra-acetic acid and urea etc. adjust solution ph as incendiary agent, optimum organization
In the range of 1~6, solution is placed in and is warmed up in 250~800 DEG C of Muffle furnace in advance, solvent combustion synthesis puffy thing
Matter, 1~4h is heat-treated at 350~800 DEG C, and one-step method obtains crystallite dimension in 5~200nm hafniums acid yttrium nanocrystalline powder.We
, compared to solid phase method and coprecipitation method, synthesis temperature is relatively low, and the time cycle is shorter, even grain size for method, can scale metaplasia
The features such as product.
The present invention prepares being mainly characterized by for the hafnium acid yttrium powder body of various grain sizes：Conventional solid reaction is overcome, is mixed
Material is uneven, the larger not easy-operating technological deficiency of sintering temperature crystallite dimension higher.The present invention is with yttrium nitrate and hafnium tetrachloride
Or oxychlorination hafnium is raw material, using the solvent combustion method in wet chemical method, solution is well mixed, and reaction temperature is relatively low, synthesis
Speed is fast, it is easy to operation and large-scale production.The preferred incendiary agent combination of the present invention, optimizes Technology for Heating Processing, and one-step method is realized
The hafnium acid yttrium nano-powder of different crystal particle scales, in one-step synthesis method, due to using different incendiary agents, the addition of incendiary agent
Amount and the firing temperature of reaction so that the crystallite dimension of the hafnium acid yttrium ceramic powder after the completion of synthesis produces change.Use
This method single sintering grain size range between 5~200nm, even grain size.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of the hafnium acid yttrium powder body of synthesis
Fig. 2 is the TEM bright field images for synthesizing hafnium acid yttrium powder body
Fig. 3 is the TEM details in a play not acted out on stage, but told through dialogues photos for synthesizing hafnium acid yttrium powder body
Specific embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment 1：
The present embodiment prepares hafnium acid yttrium powder body using combustion method.By hafnium tetrachloride (HfCl4) be dissolved in deionized water, plus
Enter excessive ammonia, then the electromagnetic agitation 30min under rotating speed 1000r/min, obtains fluffy white precipitate, then moves sediment
Enter centrifuge tube, repeatedly centrifugation (10000r, 5min)；The beaker that will fill precipitation be placed in magnetic agitation water-bath (60 DEG C,
1000r/min), excessive nitric acid is added, is heated while stirring until solution clarification.Then to addition yttrium nitrate and urine in solution
Element, heats while stirring until solution secondary clearing again, regulation solution ph is 2, six nitric hydrate yttrium ((YNO3)3·6H2O)) press
The mol ratio of Hf and Y is 1:1 carries out burdening calculation.Incendiary agent uses the calculating of urea, incendiary agent to equal perseverance principle using chemical valence,
Burdening calculation is carried out according to the desired amount of 1.6 times；It is placed in the Muffle furnace of 550 DEG C of intensification in advance and reacts, obtains puffy product,
Gained material is then heat-treated 2h at 800 DEG C, the powder average grain size for obtaining is in about 200nm.
Embodiment 2：
The present embodiment prepares hafnium acid yttrium powder body using combustion method.By hafnium tetrachloride (HfCl4) be dissolved in deionized water, plus
Enter excessive ammonia, then the electromagnetic agitation 30min under rotating speed 1000r/min, obtains fluffy white precipitate, then moves sediment
Enter centrifuge tube, repeatedly centrifugation (10000r, 5min)；The beaker that will fill precipitation be placed in magnetic agitation water-bath (60 DEG C,
1000r/min), excessive nitric acid is added, is heated while stirring until solution clarification.Then to addition yttrium nitrate and Portugal in solution
Grape sugar, heats while stirring until solution secondary clearing again, regulation solution ph is 1, six nitric hydrate yttrium ((YNO3)3·6H2O))
It is 1 by the mol ratio of Hf and Y:1 carries out burdening calculation, and incendiary agent carries out burdening calculation according to the desired amount of 1.2 times；Then by institute
Obtain presoma and be placed in the Muffle furnace of 450 DEG C of intensification in advance and react, puffy product is obtained, then by gained material at 800 DEG C
Heat treatment 2h, obtains required powder powder grain yardstick in 7~10nm.
Embodiment 3：
The present embodiment prepares hafnium acid yttrium powder body using combustion method.It is 1 by the mol ratio of Hf and Y:1 carries out burdening calculation, will
Hafnium tetrachloride (HfCl4) be dissolved in deionized water, compare 1 by mol then to yttrium nitrate, EDTA and urea is added in solution:1 mixes
It is incendiary agent to cooperate, and according to the chemical valence equilibrium principle of redox reaction, incendiary agent 1.4 times of introducings in the desired amount will be filled
The beaker of mixed solution is placed in electromagnetic agitation water-bath (60 DEG C, 1000r/min), until solution is clarified, regulation pH value is 1.Will
The beaker for filling mixed solution is placed in reaction in the Muffle furnace of 450 DEG C of intensification in advance, puffy product is obtained, then by gains
Matter is heat-treated 2h at 700 DEG C, and the powder average grain size for obtaining is in 50~100nm.
Embodiment 4：
The present embodiment prepares hafnium acid yttrium powder body using combustion method.Oxychlorination hafnium is dissolved in deionized water, is added excessive
Ammoniacal liquor, then the electromagnetic agitation 30min under rotating speed 1000r/min, obtains fluffy white precipitate, then moves into sediment and is centrifuged
Pipe, repeatedly centrifugation (10000r, 5min)；The beaker that precipitation will be filled is placed in magnetic agitation water-bath (60 DEG C, 1000r/
Min), excessive nitric acid is added, is heated while stirring until solution clarification.It is then to yttrium nitrate and mol ratio is added in solution
1：1 glycine and EDTA, heats while stirring until solution secondary clearing again, regulation solution ph is 1, is placed in intensification in advance
Reacted in 450 DEG C of Muffle furnace, obtain puffy product, gained material is then heat-treated 2h at 800 DEG C, obtain required powder
Body.
Embodiment 5：
The present embodiment prepares hafnium acid yttrium powder body using combustion method.By hafnium tetrachloride (HfCl4) be dissolved in deionized water, with
Yttrium nitrate and glycine are added in backward solution, the beaker that will fill mixed solution be placed in electromagnetic agitation water-bath (60 DEG C,
1000r/min), it is 3, six nitric hydrate yttrium ((YNO to regulation solution ph in adding solution until solution is clarified3)3·
6H2O the mol ratio for)) pressing Hf and Y is 1:1 carries out burdening calculation.Incendiary agent uses glycine, is placed in the horse of 550 DEG C of intensification in advance
Not reacted in stove, obtain puffy product, gained material is then heat-treated 4h, the powder average crystal grain chi for obtaining at 600 DEG C
It is very little in 20nm.
Claims (5)
1. the preparation method of a kind of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder, it is characterised in that step is as follows：
The preparation of step 1, presoma：By hafnium tetrachloride HfCl4Or oxychlorination hafnium is dissolved in deionized water, excess of ammonia water is added,
Obtain without Cl-The sediment of ion；Be placed in again in magnetic agitation water-bath, add excessive nitric acid, dissolution precipitation thing until
Presented in beaker and be free of Cl-The transparency liquid of ion；
Step 2：It is 1 according to Hf and Y mol ratios:1 metering than weighing yttrium nitrate, and by yttrium nitrate addition step 1 obtain it is saturating
Mixed solution is formed in prescribed liquid；
Carbon containing or nitrogenous incendiary agent is added to mixed solution, while adding ammoniacal liquor and nitric acid, regulation solution ph is 1~6；
The calculating of the incendiary agent carries out proportioning meter using the flat perseverance principle of chemical valence according to 0.6~1.6 times of the incendiary agent for being calculated
Calculate；
Step 3：The beaker of mixed solution will be filled, is placed in and is raised in the Muffle furnace that temperature is 200~800 DEG C in advance, with molten
The volatilization of agent, solution concentration constantly increases, and collosol and gel is gradually formed, and last solution combustion obtains puffy material；
Step 4：It it is 350~800 DEG C in temperature by the heat treatment of puffy material, heat treatment time is 1~4h, and it is unnecessary to remove
Carbon residue obtains the hafnium acid yttrium white powder of various grain sizes.
2. the preparation method of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder, its feature according to claim 1
It is：The step 1 is changed to：Hafnium tetrachloride or oxychlorination hafnium are directly substantially soluble in deionized water, are sufficiently stirred for being formed and are contained
Cl-The transparency liquid of ion；Then the hafnium acid yttrium white powder that step 2~step 4. obtains various grain sizes is carried out.
3. the preparation method of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder, its feature according to claim 1
It is：The incendiary agent is pure for analysis, including：Urea, citric acid, edta edta, glucose, ethanol or glycine
In one or more incendiary agents combination.
4. the preparation method of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder, its feature according to claim 1
It is：The hafnium tetrachloride HfCl4With oxychlorination hafnium HfCl2O·8H2It is pure that O is analysis.
5. the preparation method of one-step synthesis method various grain sizes hafnium acid yttrium ceramic powder, its feature according to claim 1
It is：Yttrium nitrate Y (the NO3)3·6H2O is pure or high-purity for analysis.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111908922A (en) * | 2020-08-06 | 2020-11-10 | 西北工业大学 | Low-temperature synthesized rare earth hafnate high-entropy ceramic powder and preparation method thereof |
| CN116023136A (en) * | 2023-01-19 | 2023-04-28 | 北京理工大学 | Nano-structure rare earth hafnate ceramic powder feed for thermal spraying and preparation method and application thereof |
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| CN111908922A (en) * | 2020-08-06 | 2020-11-10 | 西北工业大学 | Low-temperature synthesized rare earth hafnate high-entropy ceramic powder and preparation method thereof |
| CN116023136A (en) * | 2023-01-19 | 2023-04-28 | 北京理工大学 | Nano-structure rare earth hafnate ceramic powder feed for thermal spraying and preparation method and application thereof |
| CN116023136B (en) * | 2023-01-19 | 2024-02-09 | 北京理工大学 | Nano-structure rare earth hafnate ceramic powder feed for thermal spraying and preparation method and application thereof |
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