CN103588211A - Preparation method of spherical zirconium silicate nano aggregate powder - Google Patents
Preparation method of spherical zirconium silicate nano aggregate powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 132
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002002 slurry Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000725 suspension Substances 0.000 claims abstract description 21
- 230000006698 induction Effects 0.000 claims abstract description 18
- 239000012528 membrane Substances 0.000 claims abstract description 14
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 6
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 4
- 239000002243 precursor Substances 0.000 claims abstract 4
- 239000000084 colloidal system Substances 0.000 claims abstract 3
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract 3
- 239000002244 precipitate Substances 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 6
- 239000011858 nanopowder Substances 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- UVGLBOPDEUYYCS-UHFFFAOYSA-N silicon zirconium Chemical compound [Si].[Zr] UVGLBOPDEUYYCS-UHFFFAOYSA-N 0.000 abstract 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 15
- 239000002245 particle Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 235000010755 mineral Nutrition 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 5
- 238000000889 atomisation Methods 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 230000035508 accumulation Effects 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910006501 ZrSiO Inorganic materials 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- -1 silicate compound Chemical class 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002103 nanocoating Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000005563 spheronization Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明涉及一种硅酸锆球形纳米团聚体粉体的制备方法，属于无机材料技术领域。通过将氯氧化锆和偏硅酸钠与水混合，分离出沉淀，洗涤，干燥得前驱体；向前驱体中加氟化钠和水，在180～380℃反应4～10h，得含杂质硅酸锆粉体；将含杂质硅酸锆粉体与水混合，用无机膜分离器过滤和洗涤，得浓缩浆料，压滤得饼状粉体，干燥得硅酸锆粉体；将硅酸锆粉体与无水乙醇混合，在胶体磨中研磨、乳化，得硅酸锆纳米粉体与无水乙醇的混合悬浊液；将所述混合悬浊液用液态送粉器和感应等离子球化设备处理，对其中硅酸锆纳米粉体进行团聚、球化及致密化处理，得所述粉体。该方法简单，成本低，可直接制得硅酸锆球形纳米团聚体粉体，纯度品质得到提高。
The invention relates to a method for preparing zirconium silicate spherical nano aggregate powder, which belongs to the technical field of inorganic materials. By mixing zirconium oxychloride and sodium metasilicate with water, the precipitate is separated, washed, and dried to obtain the precursor; add sodium fluoride and water to the precursor, and react at 180-380°C for 4-10 hours to obtain impurity-containing silicon zirconium acid powder; mix impurity-containing zirconium silicate powder with water, filter and wash with an inorganic membrane separator to obtain concentrated slurry, press filter to obtain cake-shaped powder, and dry to obtain zirconium silicate powder; Mix zirconium powder with absolute ethanol, grind and emulsify in a colloid mill to obtain a mixed suspension of zirconium silicate nanopowder and absolute ethanol; use a liquid powder feeder and an induction plasma ball to prepare the mixed suspension Processing equipment, wherein the zirconium silicate nano-powder is agglomerated, spheroidized and densified to obtain the powder. The method is simple and low in cost, and the zirconium silicate spherical nano-aggregate powder can be directly prepared, and the purity and quality are improved.
Description
Technical field
The present invention relates to a kind of zirconium silicate (ZrSiO
4) preparation method of ball shaped nano coacervate powder, belong to technical field of inorganic material.
Background technology
Along with the development of Aeronautics and Astronautics technology, the use temperature of aircraft engine hot-end component and body, pressure require to improve constantly.Correspondingly, high temperature resistant, the antioxidant property for aircraft engine hot-end component and material that body is used had higher requirement.Zirconium silicate (ZrSiO
4) be a kind of silicate compound with tetragonal system island structure, zirconium white with YSZ(stabilized with yttrium oxide) compare, there is higher specific refractory power, more excellent high-temperature-phase structural stability, chemical stability (as acid-alkali-corrosive-resisting), fabulous thermal shock resistance and antioxidant property preferably, based on described advantage, make zirconium silicate material extensive in aerospace field application prospect.Ball shaped nano reunion powder can for thermospray, sintering and etc. static pressure etc. using the moulding process of powder body material as raw material.
At present, the method for preparing the original nano-powder of zirconium silicate mainly contains the several different methods such as solid phase method, the precipitator method, hydrothermal method, sol-gel method.In the preparation process of coacervate powder, the original nano-powder of zirconium silicate generally need to pass through the techniques such as calcining, mist projection granulating and high temperature sintering, after the above-mentioned art breading of process, the original nano-powder crystal grain overwhelming majority is often grown up for micron crystal grain, making the coacervate powder finally making is micron order, under in nodulizing, between a plurality of nano-powder small-particles, can stick together and become a micron spherical powder; Using zirconium silicate micron coacervate powder during as raw material, in the coating structure being made by it, have hardly nanostructure, be difficult to represent nano coating performance advantage; Meanwhile, the spherical powder surface of micron is generally relatively more loose, coarse, and bonding strength is lower, affects its use properties; And the subsequent disposal operation of prior art too much, too numerous and diverse.In view of this, in the urgent need to developing a kind of preparation method of new zirconium silicate nanoclusters aggressiveness powder, overcome above shortcoming.
Summary of the invention
For the nanocrystal existing in prior art, be difficult to the shortcoming retaining, the spherical powder surface of micron exists more defect, the object of the invention is to provide a kind of preparation method of zirconium silicate ball shaped nano coacervate powder, described method is by the adjustment to related process parameter, can obtain the surface compact of certain particle size range distribution, bright and clean, solid ball shaped nano coacervate powder, described powder has excellent flowing property, high-temperature-phase Stability Analysis of Structures, chemical stability are better, in heat barrier coat material field, have good application prospect.
The object of the invention is to be achieved through the following technical solutions.
A preparation method for zirconium silicate ball shaped nano coacervate powder, described method steps is as follows:
(1) basic zirconium chloride and Starso are mixed with water as raw material, isolate precipitation and wash, dry, obtain presoma; Wherein, the mol ratio of basic zirconium chloride and Starso is 0.8～1.5:1, and the mass ratio of water and raw material is 6～10:1;
(2) in presoma, add mineralizer Sodium Fluoride (NaF) and water to carry out hydro-thermal reaction, temperature of reaction is 180 ℃～380 ℃, and the reaction times is 4h～10h, obtains impure zirconium silicate powder; Wherein, the mol ratio of fluorine element and zr element is 2:1;
(3) impure zirconium silicate powder step (2) being obtained mixes with water, adopt mineral membrane isolation technique to filter and wash, obtain concentrated slurry, will concentrate slurry press filtration and obtain pie powder, dry, obtain zirconium silicate powder, wherein, mineral membrane isolation technique adopts inorganic diaphragm separator to carry out, working pressure is 0.15MPa～0.25MPa, wash temperature is 50 ℃～80 ℃, and the dehydration rate of concentrated slurry is 50%～70%, and the pH value of concentrated slurry is 6～8;
(4) zirconium silicate powder step (3) being obtained mixes with dehydrated alcohol, puts into that colloidal mill grinds, emulsification, obtains the suspension liquid that mixes of zirconium silicate nanometer powder body and dehydrated alcohol;
(5) zirconium silicate nanometer powder body step (4) being obtained and dehydrated alcohol mix the liquid powder feeder of suspension liquid utilization and induction plasma nodularization equipment is processed, to the zirconium silicate nanometer powder body in described suspension liquid reunite, nodularization and densification, obtain described a kind of zirconium silicate ball shaped nano coacervate powder;
Wherein, the water in step (1), (2) and (3) is water more than purity >=deionized water purity.
In step (3), the film that the separated preferably use of mineral membrane aperture is 50nm～2 μ m, working pressure is 0.2MPa, the pH value of concentrated slurry is 7; Press filtration can adopt pressure filter to carry out, and preferably the disposable material mouth through pressure filter of concentrated slurry adds it interior to 2/3 of pressure filter volume, and pressure filter internal pressure is 0.5Kg/cm
2; It is dry that pie powder can be placed in baking oven, and 5h～24h preferably dewaters at 100 ℃.
In step (4), preferably the mass ratio of zirconium silicate powder and dehydrated alcohol is 1:5～8; Preferably the rotating speed of colloidal mill is 2880r/min, and the zirconium silicate nanometer powder body now obtaining has good mobility with dehydrated alcohol mixing suspension liquid.
In step (5), utilizing liquid powder feeder and induction plasma nodularization equipment to process can adopt method specific as follows: zirconium silicate nanometer powder body is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, and the particle after atomization, after induction plasma heating, nodularization, densification occurs; In treating processes, preferably plasma power is 28KW～30KW, atomizing gas flow is 5slpm～7slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 6slpm～7slpm, argon flow amount is 50slpm～60slpm, chamber pressure is 8psia～12psia, and powder feeder rotating speed is 6r/mim～8r/mim; The zirconium silicate ball shaped nano coacervate powder surface obtaining is bright and clean, fine and close, and size distribution is 20 μ m～100 μ m.
Beneficial effect
1, the invention provides a kind of preparation method of zirconium silicate ball shaped nano coacervate powder, described method can directly prepare zirconium silicate ball shaped nano coacervate powder from the original nano-powder of zirconium silicate, not only can avoid the introducing of impurity, meanwhile, the purity of powder is improved; Described method is simple, has reduced the preparation cost of zirconium silicate ball shaped nano coacervate powder;
2. the invention provides a kind of preparation method of zirconium silicate ball shaped nano coacervate powder, described method is utilized the advantage that hydrothermal method synthesis reaction temperature is lower on the one hand, can effectively slow down the growth of zirconium silicate crystal grain, effectively avoid zirconium silicate powder generation hard aggregation, make zirconium silicate particles keep nanocrystalline structure; On the other hand, compare with calcining process with atomizing granulating technology, by using liquid powder feeding technology and induction plasma spheronization techniques to prepare fine and close zirconium silicate ball shaped nano coacervate powder, prevent the generation of defect, effectively stop the introducing of impurity, guaranteed purity and the quality of product;
In described method steps (3), preferred film aperture is 50nm～2 μ m, pressure is 0.2MPa, there is higher detersive efficiency, the median size of the concentrated slurry mesosilicic acid zirconium powder body obtaining after washing and the distribution range of particle diameter are more conducive to subsequent disposal, and this is that traditional filtration and separating technology is incomparable;
3. the invention provides a kind of preparation method of zirconium silicate ball shaped nano coacervate powder, the size distribution that described method can make is the zirconium silicate ball shaped nano coacervate powder of 20 μ m～100 μ m, mobility can reach 30s～45s/50g, can meet preferably the requirement of plasma spraying, there is not grain growth and hard aggregation phenomenon simultaneously, the primary granule particle diameter of described powder, below 100nm, maintains nanostructure in the coating that it is prepared.
Accompanying drawing explanation
Fig. 1 is the transmission electron micrograph of the zirconium silicate ball shaped nano coacervate powder primary granule for preparing of embodiment 1.
Fig. 2 is the scanning electron microscope diagram sheet of the zirconium silicate ball shaped nano coacervate powder for preparing of embodiment 1.
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of implementing the 1 zirconium silicate ball shaped nano coacervate powder preparing.
Embodiment
Below by embodiment, the invention will be further described, but embodiment does not limit the scope of the invention.
The zirconium silicate ball shaped nano coacervate powder that following examples are prepared is tested as follows:
(1) morphology observation:
Adopt NEC JEM-2100 type transmission electron microscope to observe and pattern and the size of measuring the primary granule of described powder; Adopt the pattern of coacervate powder described in the Japanese new and high technology S-4800 of Co., Ltd. type awkward silence at a meeting emission scan electron microscope observation;
(2) X-ray diffraction analysis:
X ' the Pert PRO MPD type polycrystal X ray diffraction analysis instrument that adopts Dutch PANalytical company to produce is analyzed; Test conditions: Cu target, K α, Ni filter plate; Tube voltage 40kV, tube current 40mA; Slit sizes DS=0.957 °, PSD=2.12,4 °/min of sweep velocity;
(3) mobility-detected:
The FL4-1 type device for measuring flowability that utilizes Iron and Steel Research Geueral Inst to produce detects; Testing method: the needed time of standard funnel that crosses predetermined hole diameter with flow of powder described in 50g represents.
(1) by 31.70g eight water basic zirconium chloride (ZrOCl
28H
2o), 34.97g non-hydrate sodium metasilicate (Na
2siO
39H
2o) as raw material, mix with 500g deionized water, isolate precipitation through deionized water wash, 100 ℃ of oven dryings, the powder obtaining is presoma;
(2) in 18g presoma, add 8.26g mineralizer Sodium Fluoride (NaF) to mix with 1L deionized water, insert in 1.5L cartridge type reactor and carry out hydro-thermal reaction, the reaction times is 4h, and temperature of reaction is 180 ℃, obtain impure zirconium silicate powder, now powder occurs soft-agglomerated;
(3) the impure zirconium silicate powder of the 18g obtaining in step (2) is mixed with 4L deionized water, adopt inorganic diaphragm separator to wash, filter and obtain concentrated slurry, wherein the working pressure of inorganic diaphragm separator is 0.2MPa～0.25MPa, wash temperature is 70 ℃～80 ℃, membrane pore size is 100nm, the dehydration rate of concentrated slurry is 50%～70%, and the pH value of the concentrated slurry obtaining through mineral membrane separating treatment is 7; Concentrated slurry adopts pressure filter to carry out press filtration processing, and the disposable material mouth through pressure filter of concentrated slurry adds it interior to volume 2/3, and pressure filter internal pressure is 0.5Kg/cm
2, obtain pie powder, dry through 100 ℃, baking oven, obtain zirconium silicate powder;
(4) 100g zirconium silicate powder being mixed with 500g dehydrated alcohol, put in colloidal mill, is grinding, emulsification under 2880r/min condition at rotating speed, obtains zirconium silicate nanometer powder body and dehydrated alcohol mixing suspension liquid;
(5) zirconium silicate nanometer powder body obtaining in step (4) is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, after induction plasma heating, there is nodularization in the particle after atomization, densification, the parameter of induction plasma nodularization equipment is: plasma power is 28KW, the flow of atomizing gas argon gas is 5slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 6slpm, argon flow amount is 50slpm, chamber pressure is 8psia, powder feeder rotating speed is 6r/mim, obtain a kind of zirconium silicate ball shaped nano coacervate powder of the present invention.
The zirconium silicate ball shaped nano coacervate powder that the present embodiment is prepared detects, and result is as follows:
(1) morphology microstructure:
The pattern of described powder as illustrated in fig. 1 and 2, as shown in Figure 1, obtains the floccule mass aggressiveness that a plurality of particle accumulations to piece are, and each nano particle is of a size of 10nm～25nm; As shown in Figure 2, described coacervate powder is surface compact and smooth spherical, and size distribution is 20 μ m～70 μ m;
(2) X-ray diffraction analysis:
The X ray diffracting spectrum of described powder as shown in Figure 3, meets well with the X ray diffracting spectrum (JCPD, NO.80-1807) of standard zirconium silicate, and characteristic peak all occurs, and the appearance of assorted peak, illustrates and prepares the zirconium silicate powder that purity is higher;
(3) mobility-detected:
Known after testing, the flowing property of described powder is 36s/50g.
Embodiment 2
(1) 41.98g eight water basic zirconium chlorides, 24.69g non-hydrate sodium metasilicate are made into mixing solutions as raw material and 650g deionized water, isolate precipitation through deionized water wash, 100 ℃ of oven dryings, the powder obtaining is presoma.
(2) in 24g presoma, add 10.94g mineralizer Sodium Fluoride to mix with 1L deionized water, insert 1.5L cartridge type reactor and carry out hydro-thermal reaction, the reaction times is 10h, and temperature of reaction is 380 ℃, obtain impure zirconium silicate powder, now powder occurs soft-agglomerated;
(3) the impure zirconium silicate powder of the 24g obtaining in step (2) is mixed with 4L deionized water, adopt inorganic diaphragm separator to wash, filter and obtain concentrated slurry, wherein the working pressure of inorganic diaphragm separator is 0.2MPa～0.25MPa, wash temperature is 70 ℃～80 ℃, membrane pore size is 100nm, the dehydration rate of concentrated slurry is 50%～70%, and the pH value of the concentrated slurry obtaining through mineral membrane separating treatment is 7; Concentrated slurry carries out press filtration processing through pressure filter, and the disposable material mouth through pressure filter of concentrated slurry adds it interior to volume 2/3, and pressure filter internal pressure is 0.5Kg/cm
2, obtain pie powder, dry through 100 ℃, baking oven, obtain zirconium silicate powder;
(4) 100g zirconium silicate powder being mixed with 800g dehydrated alcohol, put in colloidal mill, is grinding, emulsification under 2880r/min condition at rotating speed, obtains zirconium silicate nanometer powder body and dehydrated alcohol mixing suspension liquid;
(5) zirconium silicate nanometer powder body obtaining in step (4) is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, after induction plasma heating, there is nodularization in the particle after atomization, densification, the parameter of induction plasma nodularization equipment is: plasma power is 30KW, the flow of atomizing gas argon gas is 7slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 6slpm, argon flow amount is 60slpm, chamber pressure is 12psia, powder feeder rotating speed is 8r/mim, obtain a kind of zirconium silicate ball shaped nano coacervate powder of the present invention.
The zirconium silicate ball shaped nano coacervate powder that the present embodiment is prepared detects, and result is as follows:
(1) morphology microstructure:
The floccule mass aggressiveness that obtains a plurality of particle accumulations to piece, each nano particle is of a size of 5nm～50nm; Described coacervate powder is surface compact and smooth spherical, and size distribution is 20 μ m～80 μ m;
(2) X-ray diffraction analysis:
The X ray diffracting spectrum (JCPD, NO.80-1807) of the X ray diffracting spectrum of described powder and standard zirconium silicate meets well, and characteristic peak all occurs, and the appearance of assorted peak, illustrates and prepares the zirconium silicate powder that purity is higher;
(3) mobility-detected:
Known after testing, the flowing property of described powder is 40s/50g.
Embodiment 3
(1) by 35.42g eight water basic zirconium chlorides, 31.25g non-hydrate sodium metasilicate mixes with 500g deionized water as raw material, isolates precipitation through deionized water wash, 100 ℃ of oven dryings, and the powder obtaining is presoma;
(2) in 20g presoma, add 9.22g mineralizer Sodium Fluoride to mix with 1L deionized water, insert 1.5L cartridge type reactor and carry out hydro-thermal reaction, the reaction times is 6h, and temperature of reaction is 200 ℃, obtains impure zirconium silicate powder, and now powder occurs soft-agglomerated;
(3) the impure zirconium silicate powder of the 20g obtaining in step (2) is mixed with 4L deionized water, adopt inorganic diaphragm separator to wash, filter and obtain concentrated slurry, wherein the working pressure of inorganic diaphragm separator is 0.2MPa～0.25MPa, wash temperature is 70 ℃～80 ℃, membrane pore size is 100nm, concentrated slurry dehydration rate be 50%～70%, the pH value of the concentrated slurry obtaining through mineral membrane separating treatment is 7; Concentrated slurry carries out press filtration processing through pressure filter, and the disposable material mouth through pressure filter of concentrated slurry adds it interior to volume 2/3, and pressure filter internal pressure is 0.5Kg/cm
2, obtain pie powder, dry through 100 ℃, baking oven, obtain zirconium silicate powder;
(4) 100g zirconium silicate powder being mixed with 600g dehydrated alcohol, put in colloidal mill, is grinding, emulsification under 2880r/min condition at rotating speed, obtains zirconium silicate nanometer powder body and dehydrated alcohol mixing suspension liquid;
(5) zirconium silicate nanometer powder body obtaining in step (4) is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, after induction plasma heating, there is nodularization in the particle after atomization, densification, the parameter of induction plasma nodularization equipment is: plasma power is 29KW, the flow of atomizing gas argon gas is 6slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 7slpm, argon flow amount is 50slpm, chamber pressure is 11psia, powder feeder rotating speed is 7r/mim, obtain a kind of zirconium silicate ball shaped nano coacervate powder of the present invention.
The zirconium silicate ball shaped nano coacervate powder that the present embodiment is prepared detects, and result is as follows:
(1) morphology microstructure:
The floccule mass aggressiveness that obtains a plurality of particle accumulations to piece, each nano particle is of a size of 10nm～40nm; Described coacervate powder is surface compact and smooth spherical, and size distribution is 30 μ m～100 μ m;
(2) X-ray diffraction analysis:
The X ray diffracting spectrum (JCPD, NO.80-1807) of the X ray diffracting spectrum of described powder and standard zirconium silicate meets well, and characteristic peak all occurs, and the appearance of assorted peak, illustrates and prepares the zirconium silicate powder that purity is higher;
(3) mobility-detected:
Known after testing, the flowing property of described powder is 48s/50g.
Claims (8)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922354A (en) * | 2014-04-24 | 2014-07-16 | 北京化工大学 | High-yield zirconium silicate powder synthesized by sol-gel method |
| CN105036146A (en) * | 2015-08-28 | 2015-11-11 | 北京理工大学 | Method for preparing spherical nanometer zirconium silicate powder |
| CN105110345A (en) * | 2015-08-03 | 2015-12-02 | 景德镇陶瓷学院 | A kind of preparation method of ZrSiO4 yellow ceramic pigment doped with Pr and the product and application thereof |
| CN105236431A (en) * | 2015-08-28 | 2016-01-13 | 北京理工大学 | Preparation method of spherical nano zirconium silicate powder |
| CN108483454A (en) * | 2017-08-16 | 2018-09-04 | 漳州市安泰锆业发展有限公司 | A kind of preparation process of carrier model nanoscale zirconium silicate |
| CN110938281A (en) * | 2019-12-13 | 2020-03-31 | 北京理工大学 | A modified carbon fiber reinforced phenolic resin matrix composite material and its preparation |
| CN113929474A (en) * | 2021-12-16 | 2022-01-14 | 矿冶科技集团有限公司 | Particulate matter for thermal barrier coating, preparation method of particulate matter, thermal barrier coating and engine |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050028642A1 (en) * | 2003-08-08 | 2005-02-10 | Frank Mooney | Method and apparatus for manufacturing fine powders |
| CN1874838A (en) * | 2003-08-28 | 2006-12-06 | 泰克纳等离子系统公司 | Process for the synthesis, separation and purification of powder materials |
-
2013
- 2013-11-12 CN CN201310560189.5A patent/CN103588211A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050028642A1 (en) * | 2003-08-08 | 2005-02-10 | Frank Mooney | Method and apparatus for manufacturing fine powders |
| CN1874838A (en) * | 2003-08-28 | 2006-12-06 | 泰克纳等离子系统公司 | Process for the synthesis, separation and purification of powder materials |
Non-Patent Citations (3)
| Title |
|---|
| 白柳杨 等: "高频感应热等离子体在微细球形粉体材料准备中的应用", 《高压电技术》 * |
| 陆彩飞 等: "水热合成纳米硅酸锆工艺因素分析", 《中国粉体技术》 * |
| 陆彩飞 等: "纳米硅酸锆的水热合成", 《硅酸盐学报》 * |
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|---|---|---|---|---|
| CN103922354A (en) * | 2014-04-24 | 2014-07-16 | 北京化工大学 | High-yield zirconium silicate powder synthesized by sol-gel method |
| CN105110345A (en) * | 2015-08-03 | 2015-12-02 | 景德镇陶瓷学院 | A kind of preparation method of ZrSiO4 yellow ceramic pigment doped with Pr and the product and application thereof |
| CN105036146A (en) * | 2015-08-28 | 2015-11-11 | 北京理工大学 | Method for preparing spherical nanometer zirconium silicate powder |
| CN105236431A (en) * | 2015-08-28 | 2016-01-13 | 北京理工大学 | Preparation method of spherical nano zirconium silicate powder |
| CN105236431B (en) * | 2015-08-28 | 2017-05-10 | 北京理工大学 | A kind of preparation method of spherical nano zirconium silicate powder |
| CN108483454A (en) * | 2017-08-16 | 2018-09-04 | 漳州市安泰锆业发展有限公司 | A kind of preparation process of carrier model nanoscale zirconium silicate |
| CN110938281A (en) * | 2019-12-13 | 2020-03-31 | 北京理工大学 | A modified carbon fiber reinforced phenolic resin matrix composite material and its preparation |
| CN113929474A (en) * | 2021-12-16 | 2022-01-14 | 矿冶科技集团有限公司 | Particulate matter for thermal barrier coating, preparation method of particulate matter, thermal barrier coating and engine |
| CN113929474B (en) * | 2021-12-16 | 2022-03-04 | 矿冶科技集团有限公司 | Particulate matter for thermal barrier coating and method of making the same, thermal barrier coating and engine |
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