CN102787359B - Preparation method for calcium titanate whiskers - Google Patents
Preparation method for calcium titanate whiskers Download PDFInfo
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- CN102787359B CN102787359B CN201210318802.8A CN201210318802A CN102787359B CN 102787359 B CN102787359 B CN 102787359B CN 201210318802 A CN201210318802 A CN 201210318802A CN 102787359 B CN102787359 B CN 102787359B
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Abstract
The invention relates to a preparation method for calcium titanate whiskers. The method comprises the following steps: (1) respectively grinding a calcium-containing raw material, a titanium-containing raw material and a mineralizer to enable the particle size to be 60 mesh, and obtaining reacting raw materials after uniform mixing; (2) placing the reacting raw materials in a corundum crucible, placing the corundum crucible on a muffle, setting multi-stage warming and constant-temperature procedures, warming to 800-830 DEG C at a warming speed of 5-10 DEG C/min, calcining for 1-2.5h at constant temperature, cooling to 760-785 DEG C after 30 min or 60 min, maintain at the constant temperature for 1.5-4h, and obtaining sintering products after natural cooling; (3) adding deionized water in the sintering products, performing thermostatic waterbath soaking for 2-3h at 80 DEG C, performing suction filtration after repeated washing through the deionized water, and obtaining off-white solid pressed powder; and (4) performing blast drying on the solid pressed powder to constant weight, and obtaining the off-white calcium titanate whisker products. The preparation method is simple in process and low in cost, the production rate is about 70-75%, the obtained off-white calcium titanate whisker products are good in microcosmic appearance and high in purity, can be separated from the crucible easily and are small in industrial pollution, the mineralizer is removed easily, and the calcium titanate whisker products have application values.
Description
Technical field
The present invention relates to novel inorganic functional materials preparing technical field, particularly relate to a kind of preparation method of calcium titanate whisker.
Background technology
Whisker is a kind of with the fibrous crystals material of single crystal form growth, usually not containing the defect (crystal boundary, dislocation, hole, twin etc.) existed in conventional powder material, material diameter is at micron order, its atomic arrangement high-sequential, physical strength is approximately equal to contiguous valence f., and thus intensity is close to the theoretical value of perfect crystal.The height-oriented structure of whisker not only makes it have high strength, high-modulus and high elongation rate, but also preferably performance may be shown in electricity, light, magnetic, dielectric, heat conduction, superconduction etc., the reinforcement of ceramic base, metal matrix, polymer matrix composite can be used as, play the effect of strengthening and toughening.Manufacture the functional material of high strength, be expected to be applied to the industries such as aerospace, mechanical means, pottery, plastics, building materials.According to current grasped documents and materials, the calcium titanate with perovskite structure is a kind of important ferroelectric ceramic(s) body material.Due to lower negative temperature coefficient effect and stronger erosion resistance, matrix material that calcium titanate whisker adulterates can be utilized as heat sensitive sensor, be applied in anticorrosive sensing equipment, the work-ing life of extension device.
At present, domestic and international existing correlative study, mainly concentrates on the Synthesis and applications aspect of calcium titanate powder and particulate material, there is not yet about the relevant bibliographical information of calcium titanate whisker preparation.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of calcium titanate whisker of a kind of low cost, high yield.
For solving the problem, the preparation method of a kind of calcium titanate whisker of the present invention, comprises the following steps:
(1) calcic raw material, titaniferous materials, mineralizer being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials; The mol ratio of the calcium constituent in the titanium elements in described titaniferous materials and described calcic raw material is 1 ~ 1.2:2 ~ 2.5; The quality of described mineralizer accounts for 5% ~ 15% of the total mass of described calcic raw material and described titaniferous materials;
(2) described reaction raw materials is contained in corundum crucible, be placed in retort furnace, setting multistage heats up, constant temperature program, 800 ~ 830 DEG C are warming up to, calcining at constant temperature 1 ~ 2.5h with the temperature rise rate of 5 ~ 10 DEG C/min, then through 30min or 60min, be cooled to 760 ~ 785 DEG C, constant temperature 1.5 ~ 4h, naturally cooling, obtains sintered product;
(3) in described sintered product, add deionized water by the feed liquid mass volume ratio of 1:10, soak 2 ~ 3h in 80 DEG C of waters bath with thermostatic control, then after deionized water repetitive scrubbing suction filtration, obtain linen solid muffin;
(4) described solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain canescence calcium titanate crystal whisker products.
Described step (1) in calcic raw material be Calcium Chloride Powder Anhydrous.
Described step (1) in titaniferous materials be titanium dioxide.
Described step (1) in mineralizer be lead acetate or lime acetate.
The present invention compared with prior art has the following advantages:
1, the present invention adopts high-temperature sintering process to prepare calcium titanate whisker, product microscopic appearance better, length-to-diameter ratio and purity higher.By carrying out scanning electronic microscope (SEM to product, the JSM-5610LV type scanning electronic microscope that JEOL company of Japan produces, acceleration voltage 20 kV, operating distance 20mm, bundle spot 22, SEI) analyze, can find that products therefrom of the present invention is length 20 ~ 100 μm, be minor axis, palpus shape product, purity higher (see Fig. 1); Through XRD(Rigaku D/MAX 2500 type X-ray diffraction instrument, Cu target, 2 θ=20
°~ 80
°, electric current 200mA, voltage 40kV) to analyze, prepared crystal whisker materials chemical molecular formula is CaTiO
3, substantially (there is not raw material titanium dioxide TiO containing other impurity diffraction peak
2diffraction peak) (see Fig. 2), productive rate can reach 70 ~ 75%.
2, raw material of the present invention is easy to get, and calcining temperature is moderate, reduces production cost, and environmental pollution is less, and sintered products is easy to be separated with crucible, and product loss is less, and mineralizer is easy to wash away.
3, present invention process is simple, is suitable for industrial application.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is scanning electronic microscope (SEM) photo of calcium titanate whisker of the present invention.
Fig. 2 is X-ray diffraction (XRD) spectrogram of calcium titanate whisker of the present invention.
Embodiment
embodiment 1a preparation method for calcium titanate whisker, comprises the following steps:
(1) by 2.22g calcic raw material---Calcium Chloride Powder Anhydrous (CaCl
2), 0.80g titaniferous materials---titanium dioxide (TiO
2), 0.15g mineralizer---lead acetate (Pb (CH
3cOO)
23H
2o) being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials.
Wherein: the mol ratio of the calcium constituent in the titanium elements in titaniferous materials and calcic raw material is 1:2; The 5%(that the quality of mineralizer accounts for the total mass of calcic raw material and titaniferous materials is that pure substance calculates containing the chemical compound conversion of crystal water).
(2) contained in 25mL corundum crucible by reaction raw materials, be placed in retort furnace, be warming up to 830 DEG C, calcining at constant temperature 1h with the temperature rise rate of 5 DEG C/min, then through 30min, be cooled to 760 DEG C, constant temperature 3h, naturally cooling, obtains sintered product.
(3) in sintered product, add deionized water by the feed liquid mass volume ratio (g/mL) of 1:10, soak 2h in 80 DEG C of waters bath with thermostatic control, suction filtration after deionized water repetitive scrubbing, obtains linen solid muffin.
(4) solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain 2.11g canescence calcium titanate crystal whisker products.
As calculated, the productive rate of this calcium titanate crystal whisker products is 70.00%.
embodiment 2a preparation method for calcium titanate whisker, comprises the following steps:
(1) by 2.22g calcic raw material---Calcium Chloride Powder Anhydrous (CaCl
2), 0.88g titaniferous materials---titanium dioxide (TiO
2), 0.25g mineralizer---lead acetate (Pb (CH
3cOO)
23H
2o) being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials.
Wherein: the mol ratio of the calcium constituent in the titanium elements in titaniferous materials and calcic raw material is 1.1:2.0; The 8%(that the quality of mineralizer accounts for the total mass of calcic raw material and titaniferous materials is that pure substance calculates containing the chemical compound conversion of crystal water).
(2) contained in 25mL corundum crucible by reaction raw materials, be placed in retort furnace, be warming up to 800 DEG C, calcining at constant temperature 2.5h with the temperature rise rate of 6 DEG C/min, then be cooled to 780 DEG C through 60min, constant temperature 1.5h, naturally cooling, obtains sintered product.
(3) in sintered product, add deionized water by the feed liquid mass volume ratio (g/mL) of 1:10, soak 3h in 80 DEG C of waters bath with thermostatic control, suction filtration after deionized water repetitive scrubbing, obtains linen solid muffin.
(4) solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain 2.24g canescence calcium titanate crystal whisker products.
As calculated, the productive rate of this calcium titanate crystal whisker products is 72.30%.
embodiment 3a preparation method for calcium titanate whisker, comprises the following steps:
(1) by 2.22g calcic raw material---Calcium Chloride Powder Anhydrous (CaCl
2), 0.96g titaniferous materials---titanium dioxide (TiO
2), 0.32g mineralizer---lead acetate (Pb (CH
3cOO)
23H
2o) being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials.
Wherein: the mol ratio of the calcium constituent in the titanium elements in titaniferous materials and calcic raw material is 1.2:2.0; The 10%(that the quality of mineralizer accounts for the total mass of calcic raw material and titaniferous materials is that pure substance calculates containing the chemical compound conversion of crystal water).
(2) contained in 25mL corundum crucible by reaction raw materials, be placed in retort furnace, be warming up to 815 DEG C, calcining at constant temperature 1h with the temperature rise rate of 8 DEG C/min, then be cooled to 765 DEG C through 60min, constant temperature 4h, naturally cooling, obtains sintered product.
(3) in sintered product, add deionized water by the feed liquid mass volume ratio (g/mL) of 1:10, soak 2.5h in 80 DEG C of waters bath with thermostatic control, suction filtration after deionized water repetitive scrubbing, obtains linen solid muffin.
(4) solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain 2.27g canescence calcium titanate crystal whisker products.
As calculated, the productive rate of this calcium titanate crystal whisker products is 71.50%.
embodiment 4a preparation method for calcium titanate whisker, comprises the following steps:
(1) by 2. 50g calcic raw material---Calcium Chloride Powder Anhydrous (CaCl
2), 0.92g titaniferous materials---titanium dioxide (TiO
2), 0.41g mineralizer---lead acetate (Pb (COOH)
23H
2o) being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials.
Wherein: the mol ratio of the calcium constituent in the titanium elements in titaniferous materials and calcic raw material is 1.15:2.25; The 12%(that the quality of mineralizer accounts for the total mass of calcic raw material and titaniferous materials is that pure substance calculates containing the chemical compound conversion of crystal water).
(2) contained in 25mL corundum crucible by reaction raw materials, be placed in retort furnace, be warming up to 810 DEG C, calcining at constant temperature 2.5h with the temperature rise rate of 10 DEG C/min, then be cooled to 760 DEG C through 60min, constant temperature 1.5h, naturally cooling, obtains sintered product.
(3) in sintered product, add deionized water by the feed liquid mass volume ratio (g/mL) of 1:10, soak 3h in 80 DEG C of waters bath with thermostatic control, suction filtration after deionized water repetitive scrubbing, obtains linen solid muffin.
(4) solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain 2.44g canescence calcium titanate crystal whisker products.
As calculated, the productive rate of this calcium titanate crystal whisker products is 71.40%.
embodiment 5a preparation method for calcium titanate whisker, comprises the following steps:
(1) by 2.61g calcic raw material---Calcium Chloride Powder Anhydrous (CaCl
2), 0.96g titaniferous materials---titanium dioxide (TiO
2), 0.21g mineralizer---lime acetate (Ca (CH
3cOO)
2h
2o) being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials.
Wherein: the mol ratio of the calcium constituent in the titanium elements in titaniferous materials and calcic raw material is 1.2:2.35; The 6%(that the quality of mineralizer accounts for the total mass of calcic raw material and titaniferous materials is that pure substance calculates containing the chemical compound conversion of crystal water).
(2) contained in 25mL corundum crucible by reaction raw materials, be placed in retort furnace, be warming up to 800 DEG C, calcining at constant temperature 2h with the temperature rise rate of 5 DEG C/min, be cooled to 785 DEG C through 30min, constant temperature 2h, naturally cooling, obtains sintered product.
(3) in sintered product, add deionized water by the feed liquid mass volume ratio (g/mL) of 1:10, soak 3h in 80 DEG C of waters bath with thermostatic control, suction filtration after deionized water repetitive scrubbing, obtains linen solid muffin.
(4) solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain 2.59g canescence calcium titanate crystal whisker products.
As calculated, the productive rate of this calcium titanate crystal whisker products is 72.60%.
embodiment 6a preparation method for calcium titanate whisker, comprises the following steps:
(1) by 2.72g calcic raw material---Calcium Chloride Powder Anhydrous (CaCl
2), 0.88g titaniferous materials---titanium dioxide (TiO
2), 0.54g mineralizer---lime acetate (Ca (CH
3cOO)
2h
2o) being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials.
Wherein: the mol ratio of the calcium constituent in the titanium elements in titaniferous materials and calcic raw material is 1.10:2.45; The 15%(that the quality of mineralizer accounts for the total mass of calcic raw material and titaniferous materials is that pure substance calculates containing the chemical compound conversion of crystal water).
(2) contained in 25mL corundum crucible by reaction raw materials, be placed in retort furnace, be warming up to 815 DEG C, calcining at constant temperature 2h with the temperature rise rate of 6 DEG C/min, then be cooled to 775 DEG C through 30min, constant temperature 4h, naturally cooling, obtains sintered product.
(3) in sintered product, add deionized water by the feed liquid mass volume ratio (g/mL) of 1:10, soak 2.5h in 80 DEG C of waters bath with thermostatic control, suction filtration after deionized water repetitive scrubbing, obtains linen solid muffin.
(4) solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain 2.64g canescence calcium titanate crystal whisker products.
As calculated, the productive rate of this calcium titanate crystal whisker products is 73.30%.
embodiment 7a preparation method for calcium titanate whisker, comprises the following steps:
(1) by 2.77g calcic raw material---Calcium Chloride Powder Anhydrous (CaCl
2), 0.80g titaniferous materials---titanium dioxide (TiO
2), 0.36g mineralizer---lime acetate (Ca (CH
3cOO)
2h
2o) being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials.
Wherein: the mol ratio of the calcium constituent in the titanium elements in titaniferous materials and calcic raw material is 1.0:2.5; The 10%(that the quality of mineralizer accounts for the total mass of calcic raw material and titaniferous materials is that pure substance calculates containing the chemical compound conversion of crystal water).
(2) contain in corundum crucible by reaction raw materials, be placed in retort furnace, be warming up to 810 DEG C, calcining at constant temperature 1.5h with the temperature rise rate of 8 DEG C/min, then be cooled to 785 DEG C through 30min, constant temperature 3.5h, naturally cooling, obtains sintered product.
(3) in sintered product, add deionized water by the feed liquid mass volume ratio (g/mL) of 1:10 and soak 3h in 80 DEG C of waters bath with thermostatic control, suction filtration after deionized water repetitive scrubbing, obtains linen solid muffin.
(4) solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain 2.54g canescence calcium titanate crystal whisker products.
As calculated, the productive rate of this calcium titanate crystal whisker products is 71.20%.
embodiment 8a preparation method for calcium titanate whisker, comprises the following steps:
(1) by 2.77g calcic raw material---Calcium Chloride Powder Anhydrous (CaCl
2), 0.96g titaniferous materials---titanium dioxide (TiO
2), 0.48g mineralizer---lime acetate (Ca (CH
3cOO)
2h
2o) being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials.
Wherein: the mol ratio of the calcium constituent in the titanium elements in titaniferous materials and calcic raw material is 1.20:2.50; The 13%(that the quality of mineralizer accounts for the total mass of calcic raw material and titaniferous materials is that pure substance calculates containing the chemical compound conversion of crystal water).
(2) contain in corundum crucible by reaction raw materials, be placed in retort furnace, be warming up to 830 DEG C, calcining at constant temperature 2.5h with the temperature rise rate of 10 DEG C/min, then be cooled to 760 DEG C through 30min, constant temperature 3h, naturally cooling, obtains sintered product.
(3) in sintered product, add deionized water by the feed liquid mass volume ratio (g/mL) of 1:10, soak 3h in 80 DEG C of waters bath with thermostatic control, suction filtration after deionized water repetitive scrubbing, obtains linen solid muffin.
(4) solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain 2.80g canescence calcium titanate crystal whisker products.
As calculated, the productive rate of this calcium titanate crystal whisker products is 75.00%.
Above-mentioned reality
execute example 1 ~ 8in titanium dioxide, Calcium Chloride Powder Anhydrous, lead acetate, lime acetate be analytical reagent; High Temperature Furnaces Heating Apparatus used is beautiful really ceramic fiber retort furnace, and model is TM-0914P.
Claims (1)
1. a preparation method for calcium titanate whisker, comprises the following steps:
(1) calcic raw material, titaniferous materials, mineralizer being ground to granularity is respectively 60 orders, mixes and obtains reaction raw materials; The mol ratio of the calcium constituent in the titanium elements in described titaniferous materials and described calcic raw material is 1 ~ 1.2:2 ~ 2.5; The quality of described mineralizer accounts for 5% ~ 15% of the total mass of described calcic raw material and described titaniferous materials; Described calcic raw material is Calcium Chloride Powder Anhydrous; Described titaniferous materials is titanium dioxide; Described mineralizer is lead acetate or lime acetate;
(2) described reaction raw materials is contained in corundum crucible, be placed in retort furnace, setting multistage heats up, constant temperature program, 800 ~ 830 DEG C are warming up to, calcining at constant temperature 1 ~ 2.5h with the temperature rise rate of 5 ~ 10 DEG C/min, then through 30min or 60min, be cooled to 760 ~ 785 DEG C, constant temperature 1.5 ~ 4h, naturally cooling, obtains sintered product;
(3) in described sintered product, add deionized water by the feed liquid mass volume ratio of 1:10, soak 2 ~ 3h in 80 DEG C of waters bath with thermostatic control, then after deionized water repetitive scrubbing suction filtration, obtain linen solid muffin;
(4) described solid muffin is dried to constant weight 100 DEG C of air blast, namely obtain canescence calcium titanate crystal whisker products.
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104005080A (en) * | 2014-05-30 | 2014-08-27 | 中国科学院过程工程研究所 | Preparation method of titanium containing crystal whisker |
| CN106915766B (en) * | 2015-12-25 | 2018-01-30 | 兰州大学 | A kind of preparation method of butterfly-like shape calcium titanate particle |
| CN106241859B (en) * | 2016-08-07 | 2018-07-20 | 淮安新能源材料技术研究院 | The method for preparing solid phase of porous calcium titanate micro-nano particle ball |
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