CN113860347B - Preparation method of super-large-particle-size stable and controllable cayenne pepper-shaped calcium carbonate particles - Google Patents
Preparation method of super-large-particle-size stable and controllable cayenne pepper-shaped calcium carbonate particles Download PDFInfo
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Abstract
The application discloses a preparation method of a stable and controllable vegetable pepper-shaped calcium carbonate particle with super-large particle size, which comprises the following steps: preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent into the suspension, and uniformly stirring and mixing; the crystal form control agent is composed of ZnCl 2 And EDTA; adding a sodium carbonate solution with the concentration of 10.6g/L into the calcium hydroxide suspension by a peristaltic pump, controlling the temperature to be 60-80 ℃, and stirring at the stirring speed of 1000-1500rmb/min, and continuously stirring for 5-10min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension; and (3) filtering the calcium carbonate suspension, and drying the filter cake to obtain the capsicum-shaped calcium carbonate particles. The application provides the preparation of the vegetable pepper-shaped calcium carbonate particles with super-large particle size, stability, controllability, narrow particle size distribution and stable product, provides a direction for producing calcium carbonate with different morphologies, and is expected to widen the path for the application of the calcium carbonate; and the preparation process is simple, the production efficiency is high, the raw material sources are rich, the production cost is low, and the industrial production is easy to realize.
Description
Technical Field
The application belongs to the technical field of inorganic material preparation, and particularly relates to a preparation method of a stable and controllable cayenne pepper-shaped calcium carbonate particle with an oversized particle size.
Background
Calcium carbonate is widely used as an industrial material, and has the advantages of wide raw material sources, low price, no toxicity and harm and excellent processability. In the preparation process of the calcium carbonate, particles with different particle sizes and shapes can be obtained by adjusting reaction parameters such as temperature, reactants, additives and the like, and the particle shapes comprise cubic shapes, spindle shapes, needle shapes, spheres, chains, flakes and the like. The specific morphology and size give the calcium carbonate particles special functional applications, in particular as follows: the micron or nano spindle calcium carbonate can be applied to the fields of papermaking, hard PVC filler, paint and the like, and a certain amount of nano spindle calcium carbonate is added into the paint, so that the glossiness, the dryness, the shading force and the like of the product can be improved; spherical or hollow calcium carbonate is commonly used in the field of biological medicine because of the excellent properties of more holes, larger hole area, high solubility, good dispersibility and the like on the particle structure, and is used as a carrier of protein, DNA and biological enzyme; the nanoscale cubic-like calcium carbonate is applied to the fields of silicone adhesive, 107 adhesive, rubber and the like, and mainly plays roles of toughening, reinforcing and filling; the micron-sized needle-like or rod-like calcium carbonate is used in high-grade paper due to its high dispersibility. Based on the above, the application provides a preparation method of calcium carbonate particles with special morphology, which is expected to be applied in some special fields.
The patent CN104692437A relates to a preparation method for controllable appearance of calcium carbonate based on temperature control: introducing carbonate-containing solution or carbonate-producing gas such as CO2 or CO 2-containing gas mixture into calcium ion-containing solution at 10-100deg.C, initiating precipitation reaction, collecting precipitate after several minutes, and drying at room temperature to obtain micron-sized calcium carbonate crystals with specific morphology (chain, chrysanthemum, sphere, whisker). The appearance of the calcium carbonate prepared by the method disclosed by the application is good corresponding to the reaction temperature and is independent of the types of reactants; the prepared product has good dispersion and uniform size; and is efficient and stable in crystal form control; in addition, the temperature control method is synthesized in one step, and is simple and easy to implement. Compared with the patent, the novel calcium carbonate has the advantages that the novel calcium carbonate does not show capsicum-shaped calcium carbonate particles, and the calcium source material is calcium chloride, so that the novel calcium carbonate is low in cost and is not beneficial to industrialization.
As in patent CN105271344a, the application discloses a preparation method of calcite-shaped micron-sized calcium carbonate particles with pine cone morphology, which comprises the steps of dissolving 60 parts by weight of calcium oxide in water, preparing 5-15wt% of Ca (OH) 2 suspension by hydration reaction, adding a crystal growth composite control agent, introducing CO2 into a carbonization reaction kettle at 25-95 ℃ for primary carbonization reaction, stopping introducing CO2 when the pH value of the reaction liquid is 8-9 for secondary carbonization reaction until the pH value is 7-7.5, continuing carbonization reaction for 20min, and then conventionally filtering, washing and drying with hot air to obtain the calcite-shaped micron-sized calcium carbonate particles with pine cone morphology. The pine cone-shaped calcium carbonate product is obtained by changing the crystal growth control agent and performing the secondary carbonization reaction, has lower oil absorption value, larger surface area, and improved application effect of the calcium carbonate, and has the advantages of simple reaction condition, easy operation, lower production cost and better economic benefit, social benefit and ecological benefit.
The application relates to a method for continuously preparing petal flaky calcium carbonate crystals under the condition of supergravity field, as in patent CN 105417564A. The specific implementation steps are as follows: and (3) dropwise adding a certain amount of ammonia water into the prepared aqueous solution with the concentration of 0.005-0.02 mol/LCaCl2 to adjust the pH value, sealing and stirring, and transferring to a hypergravity reactor. The carbonization temperature is controlled to be 15-50 ℃, and CaCl rotating at high speed is arranged in a hypergravity reactor 2 The mixed solution and CO2 with the flow rate of (30-500L/h) are in countercurrent contact for carbonization reaction. When the slurry ph=6.5 to 7.0, the aeration is stopped and the carbonization reaction is ended. Centrifuging the carbonized slurry, drying at 70 ℃ for 5 hours, and crushing to obtain the petal sheet calcium carbonate product with the average particle size of 330-640 nm. Compared with other carbonization methods, the concentration of CaCl2 aqueous solution is regulated to be between 0.005 and 0.02mol/L, a crystal form control agent is not needed to be added, and the petal flaky calcium carbonate product prepared by adopting the hypergravity carbonization method has the advantages of narrower particle size distribution, uniform morphology and good dispersibility, and in addition, the carbonization time is greatly shortened.
A method for preparing calcium carbonate with different forms by using a single control agent according to the patent CN107601540a comprises the following steps: 1) Preparing sodium carbonate aqueous solution and calcium chloride aqueous solution; 2) Adding tetra sodium ethylenediamine tetraacetate into the sodium carbonate aqueous solution, and stirring and dissolving completely; 3) Slowly dripping the calcium chloride aqueous solution into the solution in the step 2) under the constant-temperature stirring condition, and continuously stirring after the reaction is completed; 4) Filtering the product obtained in the step 3), washing the product with ethanol, and drying the washed product to obtain the calcium carbonate powder. The method can realize the preparation of the micron calcium carbonate with different morphologies (spherical and spindle-shaped), can realize mass production and has good particle dispersibility. The preparation method provided by the application has the advantages of simple process flow, high solution concentration, short production period, good safety, recoverable solvent and the like.
As in patent CN108163879a, the application discloses a method for preparing calcium carbonate with different morphology and phase structure, which adopts a non-additive method, uses simple precipitation reaction of calcium acetate and sodium bicarbonate, prepares calcium carbonate particles with different morphology such as sphere, ellipsoid, petal, rod, shuttle, cube, lamellar and the like under the system of water and glycol mixed solvent, researches the influence of the concentration of calcium acetate and sodium bicarbonate, the volume ratio of water and glycol and the reaction temperature on the phase structure and morphology of the product, and the result shows that the concentration of calcium acetate and sodium bicarbonate, the volume ratio of water and glycol and the reaction temperature all influence the phase structure and morphology of calcium carbonate.
The application discloses a rugby-ball calcium carbonate and a preparation process thereof, as in patent CN109809458A, wherein the preparation method comprises the following steps: adding a crystal form guiding agent into the refined and prepared calcium hydroxide slurry, uniformly stirring, adjusting and controlling the initial carbonization temperature, introducing carbon dioxide gas to carbonize until the pH value is lower than 8, stopping, dehydrating, drying, crushing and screening to obtain the rugby-shaped calcium carbonate. The rugby-shaped calcium carbonate obtained by the application does not need surface treatment, has good dispersibility, simple process, short carbonization time and low production cost, has adjustable and controllable particle size within the range of 300-900 nanometers, has good processing fluidity as a downstream product filler, has higher added value as a template material of hollow particles, and is suitable for the light industry of foods, medicines and cosmetics, and also suitable for the industries of plastics, rubber, coatings, printing ink, papermaking, new materials and chemical industry.
The application discloses a process for preparing calcium carbonate by a bubble membrane method and application thereof, and belongs to the technical field of preparation of inorganic nonmetallic material calcium carbonate powder, as in patent CN 109824076A. The process for preparing calcium carbonate by the bubble membrane method comprises carbonization and surface treatment, wherein refined calcium hydroxide slurry is subjected to rapid carbonization reaction in a bubble membrane rapid carbonization reactor, the slurry obtained by the reaction is subjected to proper surface treatment according to the requirement, and calcium carbonate powder with uniform particle size can be obtained through filtration, drying, crushing and screening. The process for preparing the calcium carbonate by the bubble film method does not need to add a crystal form control agent, has controllable crystal morphology, uniform and controllable product particle size, good dispersibility, simple and feasible process and low production cost, and the prepared calcium carbonate powder is suitable for industries including plastics, rubber, papermaking, foods, medicines and cosmetics and has good economic and social benefits.
The application discloses a spherical calcium carbonate and a preparation method thereof, as in patent CN109824077A, wherein the preparation method comprises the following steps: slaking and aging with quicklime and water in proportion, sieving to remove impurities, adding ethanol solvent into the raw slurry, and refining and regulating to obtain calcium hydroxide slurry; transferring the prepared slurry to a hypergravity reactor, adding a crystal form control agent, and controlling carbonization temperature, CO2 gas flow and hypergravity level to enable calcium hydroxide slurry to be in countercurrent contact with carbon dioxide gas for carbonization reaction; and (3) drying and crushing the precipitate obtained after the slurry after carbonization is centrifuged to obtain the spherical calcium carbonate.
In summary, although the morphology of the calcium carbonate prepared at present is chain, spherical, rod-shaped, petal-shaped and the like, the preparation of the capsicum-like calcium carbonate particles has not been found yet.
The foregoing background is only for the purpose of providing an understanding of the inventive concepts and technical aspects of the present application and is not necessarily prior art to the present application and is not intended to be used as an aid in the evaluation of the novelty and creativity of the present application in the event that no clear evidence indicates that such is already disclosed at the date of filing of the present application.
Disclosure of Invention
The application aims to provide a preparation method of vegetable pepper-shaped calcium carbonate particles with ultra-large particle size, stability, controllability, narrow particle size distribution and stable product, which provides more morphology for the calcium carbonate particles and is expected to widen the path for the application of the calcium carbonate.
In order to achieve the above purpose, the application is realized by the following technical scheme:
a preparation method of ultra-large particle size, stable and controllable cayenne pepper-shaped calcium carbonate particles comprises the following steps:
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent into the suspension, and uniformly stirring and mixing; the crystal form control agent is composed of ZnCl 2 And EDTA groupForming;
(2) Adding a sodium carbonate solution with the concentration of 10.6g/L into the calcium hydroxide suspension by a peristaltic pump, controlling the temperature to be 60-80 ℃, and stirring at the stirring speed of 1000-1500rmb/min, and continuously stirring for 5-10min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) And (3) filtering the calcium carbonate suspension, and drying the filter cake to obtain the capsicum-shaped calcium carbonate particles.
Further, znCl in the crystal form control agent 2 And EDTA at a mass ratio of 1:1.
Further, the addition amount of the crystal form control agent is 1-5% of the mass of the calcium hydroxide.
Further, the addition rate of the sodium carbonate solution is 4-8ml/min.
Further, the drying is vacuum microwave drying.
Further, the drying is at a temperature of 80-100 ℃.
Compared with the prior art, the application has the advantages that:
the method provides the vegetable pepper-shaped calcium carbonate particles with super-large particle size, stability and controllability, narrow particle size distribution and stable product, provides a direction for producing calcium carbonate with different morphologies, and is expected to widen the path for the application of the calcium carbonate; and the preparation process is simple, the production efficiency is high, the raw material sources are rich, the production cost is low, and the industrial production is easy to realize.
Drawings
FIG. 1 is an electron microscope image of a calcium carbonate product of example 1 of the present application;
FIG. 2 is an electron microscope image of the calcium carbonate product of example 2 of the present application;
FIG. 3 is an electron microscope image of the calcium carbonate product of example 3 of the present application;
FIG. 4 is an electron micrograph of a comparative example calcium carbonate product of the present application.
Detailed Description
The technical solutions of the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
A preparation method of ultra-large particle size, stable and controllable cayenne pepper-shaped calcium carbonate particles comprises the following steps:
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 1% of the mass of calcium hydroxide into the suspension, and uniformly stirring and mixing; the crystal form control agent consists of ZnCl with the mass ratio of 1:1 2 And EDTA;
(2) Adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a rate of 8ml/min through a peristaltic pump, controlling the temperature to be 60 ℃, and stirring at a speed of 1000rmb/min, and continuously stirring for 10min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) And (3) filtering the calcium carbonate suspension, and placing the filter cake in a vacuum microwave dryer at 80 ℃ for drying to obtain the capsicum-shaped calcium carbonate particles.
The calcium carbonate prepared in the embodiment is detected by a scanning electron microscope, the detection result is shown in figure 1, the calcium carbonate prepared in the application has the shape of vegetable peppers, coarse particles, uniform distribution, particle diameters of more than 7 mu m and similar particle diameters.
Example 2
A preparation method of ultra-large particle size, stable and controllable cayenne pepper-shaped calcium carbonate particles comprises the following steps:
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 3% of the mass of calcium hydroxide into the suspension, and uniformly stirring and mixing; the crystal form control agent consists of ZnCl with the mass ratio of 1:1 2 And EDTA;
(2) Adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a rate of 5ml/min through a peristaltic pump, controlling the temperature to be 60 ℃, and stirring at a speed of 1200rmb/min, and continuously stirring for 10min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) And (3) filtering the calcium carbonate suspension, and placing the filter cake in a vacuum microwave dryer at 100 ℃ for drying to obtain the capsicum-shaped calcium carbonate particles.
The calcium carbonate prepared by the embodiment is detected by a scanning electron microscope, the detection result is shown in figure 2, the appearance of the calcium carbonate particles prepared by the application is in the shape of vegetable peppers, the particles are coarse and uniformly distributed, the particle size is larger than 5 mu m, and the particle sizes are similar.
Example 3
A preparation method of ultra-large particle size, stable and controllable cayenne pepper-shaped calcium carbonate particles comprises the following steps:
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of calcium hydroxide into the suspension, and uniformly stirring and mixing; the crystal form control agent consists of ZnCl with the mass ratio of 1:1 2 And EDTA;
(2) Adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a speed of 4ml/min through a peristaltic pump, controlling the temperature to be 80 ℃, and stirring at a speed of 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) And (3) filtering the calcium carbonate suspension, and placing the filter cake in a vacuum microwave dryer at 100 ℃ for drying to obtain the capsicum-shaped calcium carbonate particles.
The calcium carbonate prepared by the embodiment is detected by a scanning electron microscope, the detection result is shown in figure 3, the appearance of the calcium carbonate particles prepared by the application is in the shape of vegetable peppers, the particles are coarse and uniformly distributed, the particle size is larger than 5 mu m, and the particle sizes are similar.
Comparative example 1
(1) Preparing 5g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of calcium hydroxide into the suspension, and uniformly stirring and mixing; the crystal form control agent consists of ZnCl2 and EDTA in a mass ratio of 1:1;
(2) Adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a speed of 4ml/min through a peristaltic pump, controlling the temperature to be 80 ℃, and stirring at a speed of 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) And (3) filtering the calcium carbonate suspension, and placing the filter cake in a vacuum microwave dryer at 100 ℃ for drying to obtain calcium carbonate particles.
The calcium carbonate prepared in the comparative example is detected by a scanning electron microscope, the detection result is shown in figure 4, and the calcium carbonate product can be seen to obtain a clustered short bar shape; thus, the concentration of the sodium carbonate solution and the calcium hydroxide suspension has a great influence on the morphology of calcium carbonate.
Comparative example 2
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of calcium hydroxide into the suspension, and uniformly stirring and mixing; the crystal form control agent consists of ZnCl2 and EDTA in a mass ratio of 1:1;
(2) Adding 4g/L sodium carbonate solution into the calcium hydroxide suspension at a speed of 4ml/min through a peristaltic pump, controlling the temperature to be 80 ℃, and stirring at a speed of 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) And (3) filtering the calcium carbonate suspension, and placing the filter cake in a vacuum microwave dryer at 100 ℃ for drying to obtain calcium carbonate particles.
Comparative example 3
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of calcium hydroxide into the suspension, and uniformly stirring and mixing; the crystal form control agent consists of ZnCl with the mass ratio of 1:1 2 And EDTA;
(2) Adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a speed of 15ml/min through a peristaltic pump, controlling the temperature to be 80 ℃, and stirring at a speed of 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) And (3) filtering the calcium carbonate suspension, and placing the filter cake in a vacuum microwave dryer at 100 ℃ for drying to obtain calcium carbonate particles.
Comparative example 4
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of calcium hydroxide into the suspension, and uniformly stirring and mixing; the crystal form control agent consists of ZnCl2 and EDTA in a mass ratio of 1:1;
(2) Adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a rate of 1ml/min through a peristaltic pump, controlling the temperature to be 80 ℃, and stirring at a speed of 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) And (3) filtering the calcium carbonate suspension, and placing the filter cake in a vacuum microwave dryer at 100 ℃ for drying to obtain calcium carbonate particles.
The calcium carbonates prepared in examples 1 to 3 and comparative examples 1 to 4 according to the present application were measured for particle size distribution and specific surface area by a conventional method, and the measurement results are shown in Table 1.
| Sample numbering | D 50 (μm) | D 97 (μm) | BET(m 2 /g) |
| Example 1 | 9.25 | 11.50 | 1.22 |
| Example 1 | 10.76 | 12.44 | 0.98 |
| Example 1 | 8.43 | 11.32 | 1.50 |
| Comparative example 1 | 4.20 | 8.52 | 6.54 |
| Comparative example 2 | 6.27 | 14.26 | 5.31 |
| Comparative example 3 | 2.17 | 8.95 | 4.69 |
| Comparative example 4 | 8.62 | 16.22 | 8.34 |
From the test results, it was found that the concentration of the calcium carbonate solution or calcium hydroxide suspension had a great influence on the particle size of the calcium carbonate particles, and that the particle size distribution of the calcium carbonate particles obtained under the conditions of 10.6g/L of sodium carbonate solution and 8g/L of calcium hydroxide suspension was smaller and the specific surface area was larger. The addition rate of the sodium carbonate solution has great influence on the particle size distribution and specific surface area of the calcium carbonate particles, and the calcium carbonate particles prepared by the addition rate of 4-8ml/min are narrower in distribution and smaller in specific surface area.
The foregoing is a further detailed description of the application in connection with specific/preferred embodiments, and is not intended to limit the practice of the application to such description. It will be apparent to those skilled in the art that several alternatives or modifications can be made to the described embodiments without departing from the spirit of the application, and these alternatives or modifications should be considered to be within the scope of the application.
Claims (3)
1. The preparation method of the ultra-large particle size stable and controllable cayenne pepper-shaped calcium carbonate particles is characterized by comprising the following steps of:
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent into the suspension, and uniformly stirring and mixing; the crystal form control agent is composed of ZnCl 2 And EDTA;
(2) Adding a sodium carbonate solution with the concentration of 10.6g/L into the calcium hydroxide suspension by a peristaltic pump, controlling the temperature to be 60-80 ℃, and stirring at the stirring speed of 1000-1500rmb/min, and continuously stirring for 5-10min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) Filtering the calcium carbonate suspension, and drying the filter cake to obtain the capsicum-shaped calcium carbonate particles;
ZnCl in the crystal form control agent 2 And EDTA in a mass ratio of 1:1;
the adding amount of the crystal form control agent is 1-5% of the mass of calcium hydroxide;
the addition rate of the sodium carbonate solution is 4-8ml/min.
2. The method for preparing the ultra-large particle size, stable and controllable cayenne pepper-shaped calcium carbonate particles according to claim 1, which is characterized in that: the drying is vacuum microwave drying.
3. The method for preparing the ultra-large particle size, stable and controllable cayenne pepper-shaped calcium carbonate particles according to claim 2, which is characterized in that: the drying is at 80-100deg.C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1179401A (en) * | 1996-10-16 | 1998-04-22 | 长春市迪瑞检验制品有限责任公司 | Method for producing crystalline form nm-class calcium carbonate |
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| JP2007070164A (en) * | 2005-09-07 | 2007-03-22 | Nittetsu Mining Co Ltd | Silica-calcium carbonate composite particle, its producing method and pigment, filler or paper containing it |
| CN101234776A (en) * | 2007-10-31 | 2008-08-06 | 汤建新 | Process for preparing nano calcium carbonate |
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2021
- 2021-10-27 CN CN202111252458.2A patent/CN113860347B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1179401A (en) * | 1996-10-16 | 1998-04-22 | 长春市迪瑞检验制品有限责任公司 | Method for producing crystalline form nm-class calcium carbonate |
| CN1309089A (en) * | 2001-02-16 | 2001-08-22 | 清华大学 | Process for preparing nm-class calcium carbonate |
| JP2007070164A (en) * | 2005-09-07 | 2007-03-22 | Nittetsu Mining Co Ltd | Silica-calcium carbonate composite particle, its producing method and pigment, filler or paper containing it |
| CN101234776A (en) * | 2007-10-31 | 2008-08-06 | 汤建新 | Process for preparing nano calcium carbonate |
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| Title |
|---|
| The Role Of Crystal Control Agent in the Formation Of Needlelike Calcium Carbonate Nano Particles;Yuqian Ye et al.;《Advanced Materials Research》;20110512;第236-238卷;2150-2159 * |
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