CN109809482A - A kind of preparation method of monodisperse, multiform looks Zirconium powder - Google Patents
A kind of preparation method of monodisperse, multiform looks Zirconium powder Download PDFInfo
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Abstract
The invention discloses the preparation methods of a kind of monodisperse, multiform looks Zirconium powder, Zirconium powder after fluorine boron rock agent is added into zirconyl chloride solution, by regulating and controlling mineralizer concentration, through hydro-thermal method synthesis multiform looks in reaction kettle, powder dispersity is good, crystal grain is uniform, does not reunite, and size is in 50-2000nm, and synthetic method of the present invention is simple, reaction condition is mild, it is easily achieved, it is reproducible, it is at low cost.The present invention is suitable for preparing monodisperse, multiform looks Zirconium powder.
Description
Technical field
The invention belongs to field of nanometer material technology, are related to a kind of preparation method of zirconium oxide, specifically a kind of monodisperse,
The preparation method of multiform looks Zirconium powder.
Background technique
Zirconium oxide is a kind of high temperature resistant, wear-resistant, corrosion resistant inorganic non-metallic material, except being applied to traditional fire proofed wood
Outside material and ceramic paint, also it is widely used in high-tech areas such as electronic ceramics, function ceramics and structural ceramics.Ceramics
Performance it is related with the pattern of powder used and partial size, such as in the preparation of composite ceramics by fibrous powder replace graininess
Powder can be such that the intensity of ceramic material obtained increases；Such as it can make ceramics obtained using spherical powder when preparing one-component ceramic
The density of material increases；Flaky powder can be such that ceramic thermal shock resistance obtained significantly improves.
Currently, the method for preparing Zirconium powder is varied, it mainly include solid phase method, liquid phase method, vapor phase method and water
Thermal method, however the powder reuniting of first three methods preparation is serious, be unevenly distributed, crystal structure is uncontrollable, has impurity, pattern not
The problems such as controllable, and the preparation condition of hydro-thermal method is more harsh, must such as carry out at high temperature under high pressure, the morphology microstructure list of preparation
One and structural instability.Chinese invention patent CN1008997B, " production methods of flaky zirconia type fine crystals " utilize water
Thermal synthesis method is prepared using acidic aqueous solution containing SO4 2- The flaky zirconia fine crystals of ion, then at 110-350 DEG C
At a temperature of hydro-thermal process prepare four directions or cubic zirconia, however the technology is four directions by the crystal type of hydrothermal synthesis
Or cube, high-purity monoclinic phase crystal is not generated, crystal structure is unstable at room temperature, generates the size of crystal parallel direction
It is small；In addition, the reaction is carried out in sulfuric acid solution, at high cost, operational hazards are polluted the environment.Chinese invention patent
CN101696033A uses hydro-thermal method using sodium carbonate as mineralizer synthesizing flaky zirconium oxide, and the reaction is simple, easily operated, still
The Zirconium powder pattern of synthesis is single, and powder is easy to reunite.
The above research is all made of the nano zircite that a kind of method prepares a kind of pattern, can not make under a kind of process conditions
The powder of standby different-shape, such as needs to obtain the powder of different-shape, needs to change process conditions and operating condition, technique is more multiple
It is miscellaneous, and powder is easy to produce reunion in subsequent drying and processing, is unable to satisfy downstream product to crystallite dimension and pattern multiplicity
The demand of change.Therefore easily prepared monodisperse, morphology controllable and the nano powder for being not likely to produce reunion in subsequent processing are explored
The preparation method of body has great importance.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of monodisperse, multiform looks Zirconium powder, leads to
Addition fluorine boron rock agent is crossed into zirconyl chloride solution, the Zirconium powder through hydro-thermal method synthesis multiform looks, product is uniformly dispersed,
Stable structure, synthetic method is simple, and reaction condition is mild, it is easy to accomplish, it is reproducible, it is at low cost.
In order to solve the above technical problems, the technical solution used in the present invention is:
The preparation method of a kind of monodisperse, multiform looks Zirconium powder is successively carried out according to following step sequence:
(1) zirconium oxychloride aqueous solution for configuring 0.05-1.5 mol/L, is denoted as A；
(2) fluorine boron rock agent is added into A, after mixing evenly B, the molar ratio of the fluorine boron rock agent and zirconium oxychloride is 1:
2-50；
(3) B is placed in hydrothermal reaction kettle, hydro-thermal process obtains C；
(4) C is successively carried out to washing and after alcohol washes, at 110 DEG C it is dry for 24 hours, obtain Zirconium powder.
In the present invention, after zirconium oxychloride aqueous solution is added in fluorine boron rock agent, F-、B3+It is adsorbed on ZrO2Crystal primitive Zr
(OH)4Certain crystal faces on, there are also part F-OH in the substitution primitive of part-, promote Zr (OH)4Primitive is along c { 001 } face
Orientation adhesion and intercrystalline are grown nonparasitically upon another plant with the orientation in { 100 } face, and then form more appearance structures of the present invention；
In the present invention, the additional amount of mineralizer is vital for the pattern influence of Zirconium powder, when fluorine boron rock
When the molar ratio of agent and zirconium oxychloride is 1:20-50 (including 1:20), the Zirconium powder partial size of preparation is 50-300nm, pattern
For short cylinder, structure is to have pore structure；When fluorine boron rock agent and the molar ratio of zirconium oxychloride are 1:10-20 (do not include 1:
20), the Zirconium powder partial size of preparation is 200-500nm, and pattern is long column shape, and structure is to have pore structure；When fluorine boron rock agent
(1:10 is not included) when molar ratio with zirconium oxychloride is 1:5-10, the Zirconium powder partial size of preparation is 500-700nm, pattern
For pumpkin seeds shape, structure is layer structure；(do not include 1:5) when fluorine boron rock agent and the molar ratio of zirconium oxychloride are 1:2-5,
The Zirconium powder partial size of preparation is 800-2000nm, and pattern is disc shaped, and structure is layer structure.
In hydrothermal treatment process, mineralizer can participate in hydrolysis crystallization process of the zirconium oxychloride in water-heat process indirectly,
After high temperature, with water incomplete reaction occurs for zirconium oxychloride first, generates Zr (OH)4Growth unit, growth unit containing F with
Under the action of the mineralizer of B, all directions along crystal face are grown, but the size of the different crystal face speeds of growth is by OH-Free end number
How much influences；When mineralising dosage is less, syntaxic growth unit is connected first along c-axis with the face { 00l }, secondly
It is connected with the face { l00 } and { 0l0 } and the distribution that is parallel to each other, and with dehydration, forms short or long column structure；Work as mine
After agent amount increases, since the face { l00 } is the plane of symmetry of growth unit and the twin plane of monoclinic zirconia again, intercrystalline with
The face { l00 }, which is connected, to carry out orientation and grows nonparasitically upon another plant；When crystal growth, when crystal grain is grown nonparasitically upon another plant along { l00 } face orientation, the direction crystallographic axis c is to hand over
Fork, since crystal grain is fast along c-axis direction growth rate, crystal growth will carry out simultaneously in c-axis and a axis both direction, lead to powder
Bodily form looks are gradually developed from column to disc-shaped direction, and then form the zirconium oxide of different-shape.
As restriction of the invention:
In step (2), the fluorine boron rock agent borofluoride, preferably NaBF4Or NH4BF4。
In step (2), the fluorine boron rock agent is the H that weight ratio is 1:0.5-43BO3And NH4F compounds mineralizer.
In step (3), the temperature of the hydro-thermal process is 160-250 DEG C, hydrothermal conditions 1-72h；
In hydro-thermal process, the temperature of hydro-thermal reaction and time control are crucial for the formation of final Zirconium powder pattern
:
During hydro-thermal process, since crystal nucleation speed is inversely proportional with solution viscosity, the partial size of crystal of zirconium oxide with
The raising of temperature first increases to become smaller afterwards, when the temperature of hydro-thermal process is lower than 160 DEG C, Zr (OH)4Growth unit is in water-heat process
In the speed of growth it is slower, the pattern for obtaining powder will not change substantially, but the crystallization degree of powder is poor, without complete
Pattern, the easy dusting of powder, collapsing, forming degree is low；When the temperature of hydro-thermal process is higher than 250 DEG C, the powder speed of growth is accelerated,
Crystallization degree and morphology microstructure can be more regular, and solution viscosity reduces at this time, and core forming speed improves, but since nucleus quantity is led more
Solute is caused quickly to reduce the growth for being unfavorable for crystal, partial size can reduce instead at this time, cause partial size uneven, and powder is easy to roll into a ball
It is poly-.
It is less than 1h, Zr (OH) when the time of hydro-thermal process4Growth of the growth unit in water-heat process does not carry out completely, powder
The crystallization degree of body and the integrality of pattern are good not as good as long-time hydrothermal effects；It is greater than 72h when the time of hydro-thermal process, crystal is raw
The long stage has been finished, and the time extends waste of energy and time.
For the present invention there are also a kind of restriction, the Zirconium powder partial size is 50-2000nm, pattern be poroid column construction,
One of stratiform pumpkin minor structure, stratiform disc structure.
Due to the adoption of the above technical solution, compared with prior art, the present invention acquired technological progress is:
The preparation method of a kind of monodisperse provided by the invention, multiform looks Zirconium powder, by into zirconyl chloride solution plus
After entering mineralizer, by regulating and controlling mineralizer concentration, the Zirconium powder through hydro-thermal method synthesis multiform looks, powder dispersity is good, brilliant
Grain is uniform, does not reunite, and size is in 50-2000nm, and synthetic method is simple, and reaction condition is mild, it is easy to accomplish, it is reproducible,
It is at low cost.
The present invention is suitable for preparing the Zirconium powder of monodisperse, multiform looks.
The present invention is described in further detail below in conjunction with specific embodiment.
Detailed description of the invention
Fig. 1 is the XRD diagram of Zirconium powder prepared by 1- of embodiment of the present invention embodiment 5；
Fig. 2 is the SEM figure of Zirconium powder prepared by the embodiment of the present invention 1；
Fig. 3 is the SEM figure of Zirconium powder prepared by the embodiment of the present invention 2；
Fig. 4 is the SEM figure of Zirconium powder prepared by the embodiment of the present invention 3；
Fig. 5 is the SEM figure of Zirconium powder prepared by the embodiment of the present invention 4；
Fig. 6 is the SEM figure of Zirconium powder prepared by the embodiment of the present invention 5；
Fig. 7 is the XRD diagram of Zirconium powder prepared by the embodiment of the present invention 7；
Fig. 8 is the SEM figure of Zirconium powder prepared by the embodiment of the present invention 7.
Specific embodiment
The preparation method of a kind of monodisperse of embodiment 1, multiform looks Zirconium powder
The present embodiment is the preparation method of a kind of monodisperse, multiform looks Zirconium powder, it according to following step sequence successively
It carries out:
(11) zirconium oxychloride aqueous solution for configuring 0.1mol/L, is denoted as A1；
(12) mineralizer NH is added into A14BF4, after mixing evenly B1, the molar ratio of mineralizer and zirconium oxychloride are 1:25；
(13) B1 is placed in hydrothermal reaction kettle, hydro-thermal process 3h, obtains C1 at 200 DEG C；
(14) C1 is successively carried out to washing and after alcohol washes, at 110 DEG C it is dry for 24 hours, obtain Zirconium powder.
Zirconium powder manufactured in the present embodiment is subjected to XRD test and SEM test, as depicted in figs. 1 and 2, is as a result shown
Show, the Zirconium powder of preparation is in monocline phase structure, and powder is in short cylinder, and to there is pore structure；Powder long 300nm, it is wide
150nm, thick 100nm；Short cylinder monoclinic phase Zirconium powder manufactured in the present embodiment has high-specific surface area characteristic.
The preparation method of a kind of monodisperse of embodiment 2, multiform looks Zirconium powder
The present embodiment is the preparation method of a kind of monodisperse, multiform looks Zirconium powder, it according to following step sequence successively
It carries out:
(21) zirconium oxychloride aqueous solution for configuring 0.05mol/L, is denoted as A2；
(22) mineralizer NH is added into A24BF4, after mixing evenly B2, the molar ratio of mineralizer and zirconium oxychloride are 1:10；
(23) B2 is placed in hydrothermal reaction kettle, hydro-thermal process 1h, obtains C2 at 220 DEG C；
(24) C2 is successively carried out to washing and after alcohol washes, at 110 DEG C it is dry for 24 hours, obtain Zirconium powder.
Zirconium powder manufactured in the present embodiment is subjected to XRD test and SEM test, as shown in figures 1 and 3, is as a result shown
Show, the Zirconium powder of preparation is in monocline phase structure, tests and finds through SEM, and powder is in long column shape, and has pore structure.Powder
Long 540nm, wide 340nm, thick 120nm；Long column shape monoclinic phase Zirconium powder manufactured in the present embodiment has good photocatalysis
Property characteristic.
The preparation method of a kind of monodisperse of embodiment 3, multiform looks Zirconium powder
The present embodiment is the preparation method of a kind of monodisperse, multiform looks Zirconium powder, it according to following step sequence successively
It carries out:
(31) zirconium oxychloride aqueous solution for configuring 1.5mol/L, is denoted as A3；
(32) mineralizer NaBF is added into A34, after mixing evenly B3, the molar ratio of mineralizer and zirconium oxychloride are 1:5；
(33) B3 is placed in hydrothermal reaction kettle, hydro-thermal process for 24 hours, obtains C3 at 250 DEG C；
(34) C3 is successively carried out to washing and after alcohol washes, at 110 DEG C it is dry for 24 hours, obtain Zirconium powder.
Zirconium powder manufactured in the present embodiment is subjected to XRD test and SEM test, as shown in Figure 1 and Figure 4, is as a result shown
Show, the Zirconium powder of preparation is in monocline phase structure, tests and finds through SEM, and powder is in pumpkin seeds shape, and has layer structure.
Powder long 600nm, wide 400nm, thick 150nm；Pumpkin seeds shape monoclinic phase Zirconium powder manufactured in the present embodiment has good
Antiwear characteristic.
The preparation method of a kind of monodisperse of embodiment 4, multiform looks Zirconium powder
The present embodiment is the preparation method of a kind of monodisperse, multiform looks Zirconium powder, it according to following step sequence successively
It carries out:
(41) zirconium oxychloride aqueous solution for configuring 1.5mol/L, is denoted as A4；
(42) H that molar ratio is 1:2 is added into A43BO3And NH4The compounding mineralizer of F composition, compounds mineralizer and oxychlorination
The molar ratio of zirconium is 1:3, obtains B4 after mixing evenly；
(43) B4 is placed in hydrothermal reaction kettle, hydro-thermal process 72h, obtains C4 at 160 DEG C；
(44) C4 is successively carried out to washing and after alcohol washes, at 110 DEG C it is dry for 24 hours, obtain Zirconium powder.
Zirconium powder manufactured in the present embodiment is subjected to XRD test and SEM test, as shown in Figure 1 and Figure 5, is as a result shown
Show, the Zirconium powder of preparation is in monocline phase structure, tests and finds through SEM, and powder is in disc shaped, and has layer structure.Powder
Body is 2 μm, wide 1.7nm, thick 200nm long；Disc shaped monoclinic phase Zirconium powder manufactured in the present embodiment have preferable antidetonation and
It is anti-wear.
5 comparative experiments of embodiment
0.1mol/L zirconyl chloride solution is configured, NaBF is added into solution4(NaBF after being sufficiently mixed4With zirconium oxychloride mole
Than for 1:1), liquid is poured into hydrothermal reaction kettle, for 24 hours in 200 DEG C of hydro-thermal process, gained is precipitated after washing alcohol washes several times,
Drying for 24 hours, obtains powder at 110 DEG C.
The above-mentioned powder of gained is tested by XRD and SEM, as shown in Figure 1 and Figure 5, powder is no longer Zirconium powder,
But become sodium fluozirconate Na2ZrF6, this is primarily due to F in mineralizer-Concentration it is sufficiently high when, OH in solution-Do not occurring
Hydrolysis, former Zr-OH key, so the powder finally prepared is converted, generate sodium fluozirconate replaced Zr-F key
Na2ZrF6.It tests and finds through SEM, powder hexagon monocrystalline in the form of sheets.
The selection of 6 mineralizer of embodiment is probed into
During hydro-thermal reaction prepares Zirconium powder, mineralizer can be improved solubility of the solute in hydrothermal solution,
Crystal growth rate is influenced, the structure of crystal growth primitive is changed, the type of mineralizer selects the shape to final Zirconium powder
Looks are affected.The present embodiment has carried out Experimental Research, the preparation step and embodiment 1 of zirconium oxide to different mineralizer selections
Similar, the difference is that only: the type of mineralizer is different in preparation process.Concrete outcome see the table below.
First group: mineralizer provided by embodiment 1；
Second group: NaOH；
Third group: H3BO3
4th group: NH4F；
5th group: NaCO3。
By above table, it can be concluded that, only first group can just prepare Zirconium powder as described in the present invention, other
The mineralizer of classification can not prepare zirconium oxide as described in the present invention.This is primarily due to be usually used in hydrothermal synthesis zirconium oxide
The growth unit of zirconium oxide in water-heat process after this kind of mineralizer is added based on Na salt with cubic phase oxidation in the mineralizer of powder
Based on zircon-structure, tetragonal zircite is grown to isotropism, therefore obtained powder is mostly subsphaeroidal, and dispersibility is poor, easily rolls into a ball
Poly-, particle is uneven.When only containing F in mineralizer-When, orientation adhesion will not occur between powder granule and orientation is grown nonparasitically upon another plant, particle
Only individualism.When only containing B in mineralizer3+When, growth unit can occur orientation and grow nonparasitically upon another plant, but particle size does not contain with mineralizer
Amount increases and changes, and crystalline size maintains within 100nm always.And works as in mineralizer and exist simultaneously F-And B3+When, hydro-thermal is closed
At F in the process-And B3+It acts synergistically, joint effect growth unit orientation adhesion and orientation are grown nonparasitically upon another plant, crystal of zirconium oxide growth
Anisotropy, the zirconium oxide size finally prepared is controllable, and pattern multiplicity, stability is good, and particle is uniform.
7 presoma of embodiment is to ZrO2The influence of appearance
Compound concentration is 0.1 mol/L ZrOCl2·8H2O solution, is added polyethylene glycol in the solution, delays into mixed solution
It is slow to instill ammonium hydroxide (concentration 12-14%), until pH is 10, generate white flock precipitate；NaBF is added into turbid solution4Mineralizer
After be packed into reaction kettle, the molar ratio of mineralizer and zirconium oxychloride is 1:10；The hydro-thermal reaction 1h at 220 DEG C, product through washing and
After alcohol is washed, dried for 24 hours at 110 DEG C.
The above-mentioned powder of gained is tested by XRD and SEM, as shown in Figure 7 and Figure 8, the results show that the zirconia powder of preparation
Body is in monocline phase structure, tests and finds through SEM, and powder is in subsphaeroidal shape, and for powder granule having a size of nanoscale, particle is uneven,
Reunite serious.
The preparation method of embodiment 8-13 monodisperse, multiform looks Zirconium powder
Embodiment 8-13 is respectively the preparation method of a kind of monodisperse, multiform looks Zirconium powder, preparation step and 1 phase of embodiment
Seemingly, the difference is that only: corresponding technical parameter is different in preparation process, specific as follows:
Embodiment 1-4 and 8-13, are only presently preferred embodiments of the present invention, are not other forms made for the present invention
It limits, any person skilled in the art is changed or be modified as enlightenment possibly also with above-mentioned technology contents equivalent
The equivalent embodiment of variation.But all technical spirits without departing from the claims in the present invention, the letter to made by above embodiments
Single modification, equivalent variations and remodeling, still fall within the range of the claims in the present invention protection.
Claims (5)
1. the preparation method of a kind of monodisperse, multiform looks Zirconium powder, it is characterised in that successively according to following step sequence
It carries out:
(1) zirconium oxychloride aqueous solution for configuring 0.05-1.5 mol/L, is denoted as A；
(2) fluorine boron rock agent is added into A, after mixing evenly B, the molar ratio of the fluorine boron rock agent and zirconium oxychloride is 1:
2-50；
(3) B is placed in hydrothermal reaction kettle, hydro-thermal process obtains C；
(4) C is successively carried out to washing and after alcohol washes, at 110 DEG C it is dry for 24 hours, obtain Zirconium powder.
2. the preparation method of a kind of monodisperse according to claim 1, multiform looks Zirconium powder, it is characterised in that: step
Suddenly in (2), the fluorine boron rock agent is borofluoride.
3. the preparation method of a kind of monodisperse according to claim 1, multiform looks Zirconium powder, it is characterised in that: step
Suddenly in (2), the fluorine boron rock agent is the H that molar ratio is 1:0.5-43BO3And NH4F compounds mineralizer.
4. the preparation method of a kind of monodisperse according to claim 1, multiform looks Zirconium powder, it is characterised in that: step
Suddenly in (3), the temperature of the hydro-thermal process is 160-250 DEG C, hydrothermal conditions 1-72h.
5. the preparation method of a kind of monodisperse, multiform looks Zirconium powder described in any one of -4 according to claim 1,
Be characterized in that: the Zirconium powder partial size is 50-2000nm, and pattern is poroid column construction, stratiform pumpkin minor structure or layer
One of shape disc structure.
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