WO2015007011A1 - 一种自修复水泥基材料的制备方法 - Google Patents

一种自修复水泥基材料的制备方法 Download PDF

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WO2015007011A1
WO2015007011A1 PCT/CN2013/082511 CN2013082511W WO2015007011A1 WO 2015007011 A1 WO2015007011 A1 WO 2015007011A1 CN 2013082511 W CN2013082511 W CN 2013082511W WO 2015007011 A1 WO2015007011 A1 WO 2015007011A1
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cement
carrier
calcium
based material
repair
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PCT/CN2013/082511
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French (fr)
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钱春香
任立夫
荣辉
李瑞阳
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东南大学
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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
    • C12N1/20—Bacteria; Culture media therefor
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/10—Coating or impregnating
    • C04B20/1003—Non-compositional aspects of the coating or impregnation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00663—Uses not provided for elsewhere in C04B2111/00 as filling material for cavities or the like
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/72—Repairing or restoring existing buildings or building materials

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  • the invention belongs to the cross-scientific technology in the field of microbiology and building materials, and relates to a novel microbial crack repairing technology.
  • Cement concrete is currently the most widely used building material.
  • cancer the cracking problem
  • inorganic material repair and organic matter repair are widely used, inorganic materials such as grouting repair are simple but the repair effect is not satisfactory.
  • organic matter repair can obtain better results, the durability of organic matter restricts its application. And most organics do not have environmentally friendly properties.
  • Microbial self-repairing concrete is a new type of intelligent material with self-sensing and self-repairing.
  • the microbial remediation agent is embedded in the interior of the cement-based material. When cracking occurs, the microorganisms induce the formation of ore after the water and air enter. The material crack area is filled, which has the advantages of self-adaptation, self-repair, self-repair and environmental friendliness compared with the traditional repair method.
  • the present invention provides a method for repairing cracks in cement-based materials that is faster to repair.
  • the method for repairing cracks in a cement-based material of the present invention comprises the following steps:
  • the calcium source is evenly buried in the cement-based material, and the calcium source accounts for 2% to 5% of the cement material in the cement-based material, and the carrier carrying the concentrated bacteria solution of Bacillus licheniformis is concentrated in the test piece. Within 5 mm below the surface area, the carrier accounts for 10% to 20% by mass of the cementitious material.
  • the calcium source in the present invention is calcium chloride, calcium nitrate or calcium lactate.
  • the calcium source When molding the cement-based material, the calcium source is uniformly buried inside the cement-based material, the quality of the calcium source accounts for 2% to 5% of the cementitious material, and the carrier carrying the bacteria is concentrated in the range of 5 mm below the surface area of the test piece, and the carrier quality It accounts for 10% ⁇ 20% of cementitious materials.
  • the test piece After the test piece is cured, cracks are artificially made, placed in a constant temperature water bath, and continuously air-conditioned. The results of the repair test showed that after 5 days of repair, the permeability coefficient was greatly reduced, and the crack was completely repaired for 30 days.
  • the invention has the following advantages:
  • the microorganism can automatically perceive the generation of cracks, induce mineral production at the cracking point in time, and realize active repair;
  • the present invention Compared with the existing microbial repairing cement-based material cracking technology - using Bacillus licheniformis to decompose the substrate calcium lactate to induce mineral production, the present invention fully utilizes carbonic anhydrase microorganisms to capture CO 2 and promote CO 2 to CO 3 2- Conversion, accelerated carbonate mineralization, compared with the two techniques of repairing cracks under the same conditions, the effect of repairing 1 ⁇ 3d with Bacillus licheniformis is equivalent to that of Bacillus bacillus repairing 5 ⁇ 10d, and repairing cracks is faster.
  • the present invention finds in a variety of calcium sources that can be determined by calcium ion deposition test.
  • the present invention uses calcium lactate to act as a calcium source, it has a faster calcium ion deposition rate, and calcium lactate is preferred as a calcium source. Compared to other calcium sources, faster carbonate deposition rates and more carbonate precipitation can be achieved, and cracks are repaired more quickly.
  • the present invention concentrates the ceramsite immobilized with bacteria on the surface area of the cement-based material, which is different from the conventional uniform distribution in the cement-based material; the current experimental research shows that the microbial repair agent is below the surface of the crack when repairing the crack.
  • the effect of inducing ore-repairing cracks in the depth range of 2mm is obvious.
  • the repair effect of microbial repairing agent is not obvious when the crack depth exceeds 5mm.
  • the conventional method is to distribute the repairing agent evenly on the whole material, and the non-surface area microbial repairing agent can not play its role, resulting in the repairing agent.
  • Waste; the ceramsite immobilized with bacteria is concentrated on the surface area of the material, on the one hand, reducing the amount of the repair agent carrier, reducing the influence of the lightweight aggregate carrier on the mechanical properties of the cement-based material, and on the other hand, concentrating a large amount of microbial repair agent on the surface of the material, Strengthen the repair effect and repair the crack faster.
  • Figure 1 shows the trend of the permeability coefficient of the cracked specimens with the repair time without the use of this repair method (control group) and the repair method (test group).
  • Figure 2 shows the XRD pattern of the mineralized product in the fracture area when the repair method is used to repair the crack.
  • Figure 3 is an SEM image of the mineralized product of the fracture area when the repair method is used to repair the crack.
  • Fig. 4 is a graph showing changes in calcium ion concentration with time under the same conditions, maintaining the same initial calcium ion concentration, dissolving different calcium sources in an equal amount of the same concentration of Bacillus licheniformis.
  • Figure 5a shows the initial state of the crack when this repair method is not used.
  • Figure 5b shows the filling of the crack surface area when the repair method is not used.
  • Figure 5c shows the filling condition of the crack surface area when the repair method is not used for 30d.
  • Figure 6a shows the initial state of the crack when this repair method is used.
  • Figure 6b shows the filling condition of the crack surface area when the repair method is used for 5d.
  • Fig. 6c shows the filling condition of the crack surface area when the repair method is used for 30d.
  • Bacillus bacillus used in the present invention (Bacillus Mucilaginous) is from the China Industrial Microbial Culture Collection, number 21698.
  • the method for repairing cracks of cement-based materials of the invention is as follows:
  • Bacillus mucilaginous concentrated bacterial solution Bacillus mucilaginous is inoculated into the sterilized medium solution, and each liter of the medium contains sucrose 8-12 g, Na 2 HPO 4 • 12H 2 O 2 ⁇ 3g, MgSO 4 0.4 ⁇ 0.6g, CaCO 3 0.5 ⁇ 1.5g, KCl 0.1 ⁇ 0.2g, (NH 4 ) 2 SO 4 0.4 ⁇ 0.6g, yeast extract 0.2 ⁇ 0.4g, and pH control For 7 ⁇ 8, shake culture at 30 ⁇ 37 °C for 24h to obtain Bacillus mucilaginous bacteria solution. After centrifugation at 6000 ⁇ 8000 rpm for 10 ⁇ 15min at 4°C, remove the upper culture medium. Deionized water was added to the material, and the concentration of the bacteria contained in the concentrated bacterial solution was 10 6 to 10 7 /mL.
  • Calcium source, calcium nitrate or calcium lactate can be used for calcium source.
  • calcium ion deposition test is carried out: three groups of test groups are set, respectively, calcium chloride and nitric acid are taken. Calcium and calcium lactate were fully dissolved in the same concentration of Bacillus licheniformis. The initial Ca 2+ concentration in the three groups of bacteria was the same, and the culture was shaken by exposure to air. The concentration of Ca 2+ in each group was measured within 7 days. Measured every 1d over time. The results showed that the calcium ion concentration in the calcium lactate group decreased faster than that in the calcium chloride group and the calcium nitrate group.
  • the curve of Ca 2+ concentration in each group over time in 7d is shown in Figure 4.
  • the bacteria are immobilized on the carrier, the carrier is ceramsite, and the particle size is 0.6-0.3 mm.
  • the method is to soak the ceramsite in the concentrated bacteria solution of Bacillus licheniformis for 16-24 hours, and the glial spore
  • the ratio of the concentrated bacteria solution to the carrier is 50mL: 100g ⁇ 100 mL: 200 g.
  • Figure 1 shows that the permeability coefficient after 5d repaired by this repair method is similar to that after 30d maintenance without this repair method. After repairing for 30 days, almost no water seepage occurs after repair.
  • Figure 2 shows that the mineralized product is calcium carbonate.
  • Figure 3 shows the microscopic morphology of mineralized products.

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Abstract

一种自修复水泥基材料的制备方法，包括：将胶质芽孢杆菌接种至培养基培养后制备胶质芽孢杆菌浓缩菌液；将细菌固载于载体；成型水泥基材料时把钙源均匀埋入水泥基材料内部；将固载有细菌的载体集中在试件表面区域以下5m范围内。所述方法利用碳酸酐酶微生物产生碳酸酐酶捕捉CO2，促进CO2转化为CO3 2—，加速裂缝表面区域碳酸钙的沉积，较其它微生物修复裂缝具有更快的修复速度。

Description

[根据细则37.2由ISA制定的发明名称]　一种自修复水泥基材料的制备方法 技术领域
本发明属于微生物学领域和建筑材料领域的交叉科学技术，涉及一种新型微生物裂缝修复技术。
背景技术
水泥混凝土是目前应用最为广泛的建筑材料，在造成水泥混凝土耐久性下降的众多因素中，开裂问题堪称水泥混凝土的“癌症”并始终困扰着众多水泥混凝土研究人员。虽然传统的修复方法如无机物修复、有机物修复等方法应用广泛，无机物修复如灌浆修复虽工艺简便但修复效果并不理想，有机物修复虽能获得较好效果，但有机物耐久性问题制约其应用，且大多有机物并不具有环境友好特性。
微生物自修复混凝土是一种具有自感知和自修复的新型智能材料，将微生物修复剂预埋入水泥基材料内部，当发生开裂时，微生物在水和空气进入后诱导产矿的形成对水泥基材料裂缝区域进行填充，与传统修复方法相比，其有着自适应、自检测、自修复和环境友好等优点。
 技术问题
本发明提供一种修复速度更快的用于修复水泥基材料裂缝的方法。
技术解决方案
本发明的用于修复水泥基材料裂缝的方法，包括以下步骤：
1）将胶质芽孢杆菌接种至培养基培养中，制备菌体浓度为106~107个/mL的胶质芽孢杆菌浓缩菌液；
2）将载体浸泡在制备得到的胶质芽孢杆菌浓缩菌液中16~24h，使胶质芽孢杆菌固载于载体中，载体为粒径在0.6~0.3mm的陶粒，浓缩菌液和载体的配比为50mL:100g~ 100mL:200g；
3）把钙源均匀埋入水泥基材料内部，钙源占水泥基材料中胶凝材料的质量百分比为2%~5%，将固载有胶质芽孢杆菌浓缩菌液的载体集中在试件表面区域以下5mm范围内，载体占胶凝材料的质量百分比为10%~20%。
本发明中的钙源为氯化钙、硝酸钙或乳酸钙。
成型水泥基材料时把钙源均匀埋入水泥基材料内部，钙源质量占胶凝材料2%~5%，并将固载有细菌的载体集中在试件表面区域以下5mm范围内，载体质量占胶凝材料10%~20%。待试件固化后人工制作裂缝，放入恒温水浴，并持续通入空气养护。修复试验结果表明，修复5d，渗透系数大大降低，连续修复30d，裂缝完全修复。
 有益效果
本发明与现有技术相比，具有以下优点：
1、与传统的被动修复技术相比，微生物能自动感知裂缝的产生，及时在开裂处诱导产矿，从而实现主动修复；
2、与目前常用的有机类材料修复水泥基材料裂缝相比，微生物诱导矿化发生修复裂缝产生的碳酸钙以方解石形式存在，化学性质较稳定，确保了裂缝修补区域材料的耐久性，修复过程碳酸酐酶微生物吸收温室气体CO2，减缓温室效应。
3、与已有微生物修复水泥基材料裂缝技术—采用巴氏芽孢杆菌分解底物乳酸钙诱导产矿相比，本发明充分利用碳酸酐酶微生物捕捉CO2，促进CO2向CO3 2-的转化，加速碳酸盐矿化，同等条件下两种修复裂缝技术相比，采用胶质芽孢杆菌修复1~3d效果与巴氏芽孢杆菌修复5~10d效果相当，修复裂缝更快速。
4、本发明在多种可选用钙源中，通过钙离子沉积试验探明，本发明采用胶质芽孢杆菌作用乳酸钙时，具有更快的钙离子沉积速率，优先选用乳酸钙作为钙源，相比其他钙源，能获得更快的碳酸盐沉积速率和更多的碳酸盐沉淀量，修复裂缝更快速。
5、本发明将固载有细菌的陶粒集中在水泥基材料表面区域，与常规的均匀分布在水泥基材料整体不同；目前试验研究表明，微生物修复剂在修复裂缝时，在裂缝表面区域以下2mm深度范围内诱导产矿修复裂缝效果明显，裂缝深度超过5mm微生物修复剂修复效果不明显，常规方式是将修复剂均匀分布于材料整体，非表面区域微生物修复剂无法发挥作用，造成修复剂的浪费；将固载有细菌的陶粒集中在材料表面区域，一方面减少修复剂载体用量，减轻轻骨料载体对水泥基材料力学性能的影响，另一方面集中大量微生物修复剂于材料表面，强化修复效应，修复裂缝更快速。
 附图说明
图1为不采用此修复方法（对照组）和采用此修复方法（试验组）下开裂试件渗透系数随修复时间变化趋势。
图2为采用此修复方法修复裂缝时裂缝区域矿化产物XRD图谱。
图3为采用此修复方法修复裂缝时裂缝区域矿化产物SEM图。
图4为在相同条件下，保持相同初始钙离子浓度，将不同钙源溶于等量等浓度胶质芽孢杆菌菌液中培养，钙离子浓度随时间变化曲线图。
图5 a为未采用此修复方法时裂缝初始状态。
图5 b为未采用此修复方法时养护5d时裂缝表面区域填充状况。
图5 c为未采用此修复方法时养护30d时裂缝表面区域填充状况。
图6 a为采用此修复方法时裂缝初始状态。
图6 b为采用此修复方法时修复5d时裂缝表面区域填充状况。
图6 c为采用此修复方法时修复30d时裂缝表面区域填充状况。
 本发明的实施方式
本发明所用的胶质芽孢杆菌（Bacillus mucilaginous）来源于中国工业微生物菌种保藏中心，编号为21698。
本发明用于修复水泥基材料裂缝的方法，方法步骤如下：
（1）获取胶质芽孢杆菌（Bacillus mucilaginous）浓缩菌液：将胶质芽孢杆菌（Bacillus mucilaginous）接种于灭菌后的培养基溶液，每升培养基含有蔗糖8~12g、Na2HPO4•12H2O 2~3g、MgSO4 0.4~0.6g、CaCO3 0.5~1.5g、KCl 0.1~0.2g、(NH4)2SO4 0.4~0.6g、酵母提取物 0.2~0.4g，并控制pH为7~8，于30~37℃下振荡培养24h，得到含有胶质芽孢杆菌（Bacillus mucilaginous）的菌液，在4℃下经6000~8000 rpm高速离心10~15min后，除去上层培养基营养物质后加去离子水，浓缩菌液中所含菌体浓度为106~107个/mL。
（2）钙源选取：钙源选用氯化钙、硝酸钙或乳酸钙均可，为探究最佳钙源选取方案，进行钙离子沉积试验：设置三组试验组，分别取氯化钙、硝酸钙和乳酸钙于等量等浓度胶质芽孢杆菌菌液中充分溶解，三组别菌液中初始Ca2+浓度相同，暴露在空气环境下振荡培养，测量7d内各组别Ca2+浓度随时间变化情况，每隔1d测量一次。试验结果表明：乳酸钙组全程钙离子浓度随时间下降均比氯化钙组和硝酸钙组快，7d乳酸钙组钙离子浓度下降率达58.4%，7d实际产生沉淀量为0.4176g；氯化钙组、硝酸钙组钙离子浓度下降率分别为27.5%和39.4%，7d实际产生沉淀量分别为0.2495g和0.2624g；表明选用乳酸钙可获取更快的钙离子沉积速率和更多的碳酸钙沉淀量。7d内各组别Ca2+浓度随时间变化曲线具体见图4。
（3）固载细菌：将细菌固载于载体，载体为陶粒，粒径为0.6~0.3mm，其方法是将陶粒于胶质芽孢杆菌浓缩菌液中浸泡16~24h，胶质芽孢杆菌浓缩菌液和载体的配比为50mL:100g~ 100mL:200g。
（4）成型水泥基材料：成型水泥基材料时把钙源均匀埋入水泥基材料内部，钙源质量占胶凝材料2%~5%，并将固载有细菌的载体集中在试件表面区域以下5mm范围内，载体质量占胶凝材料10%~20%。
（5）养护修复：待试件固化后人工制作裂缝，放入恒温水浴，并持续通入空气养护。修复试验结果表明，修复5d，渗透系数大大降低，连续修复30d，裂缝完全修复。
图1中显示采用此修复方法修复5d后渗透系数与不采用此修复方法养护30d后渗透系数相近，采用此修复方法修复30d后几乎无渗水发生。
图2显示矿化产物为碳酸钙。
图3显示矿化产物微观形态。
实施例1：
（1）称取蔗糖12g、Na2HPO4•12H2O 3g、MgSO4 0.6g、CaCO3 1.5g、KCl 0.2g、(NH4)2SO4 0.6g、酵母提取物0.4g于1000mL去离子水中溶解，配置成所需培养基溶液，调节pH为7，125℃高温下灭菌25分钟后取出待冷却，将胶质芽孢杆菌接种至冷却培养基溶液中，30℃下振荡培养，振荡频率为170 r/min，培养时间24h；
（2）将培养好的菌液高速离心10min，离心机转速为8000 rpm，温度为4℃，去除上层培养基营养物质，加去离子水100mL制成浓缩菌液；
（3）取陶粒200g浸泡于100mL胶质芽孢杆菌（Bacillus mucilaginous）浓缩菌液中24h待用，成型水泥基材料水胶比W/C=0.36，胶凝材料用量1300g，称量20g无水氯化钙与胶凝材料混合均匀，采用内径Ф为110mm，高H为45mm的塑料圆柱形试模成型，装模过程将固载有细菌的陶粒集中分布在材料上下表面区域以下5mm范围内；
（4）待试件固化后人工制作裂缝，放入恒温水浴，并持续通入空气养护修复。
修复5d后，裂缝得到较大程度填充，渗透系数大大降低，连续修复30d，裂缝修复完全，达到优异的修复效果。
实施例2：
（1）称取蔗糖9.6g、Na2HPO4•12H2O 2.4g、MgSO4 0.48g、CaCO3 1.2g、KCl 0.16g、(NH4)2SO4 0.48g、酵母提取物0.32g于800mL去离子水中溶解，配置成所需培养基溶液，调节pH为7，125℃高温下灭菌25分钟后取出待冷却，将胶质芽孢杆菌接种至冷却培养基溶液中，30℃下振荡培养，振荡频率为170 r/min，培养时间24h；
（2）将培养好的菌液高速离心10min，离心机转速为8000 rpm，温度为4℃，去除上层培养基营养物质，加去离子水80mL制成浓缩菌液；
（3）取陶粒150g浸泡于80mL胶质芽孢杆菌（Bacillus mucilaginous）浓缩菌液中24h待用，成型水泥基材料水胶比W/C=0.36，胶凝材料用量1300g，称量40g四水硝酸钙与胶凝材料混合均匀，采用内径Ф为110mm，高H为45mm的塑料圆柱形试模成型，装模过程将固载有细菌的陶粒集中分布在材料上下表面区域以下5mm范围内；
（4）待试件固化后人工制作裂缝，放入恒温水浴，并持续通入空气养护修复。
修复5d后，裂缝得到较大程度填充，渗透系数大大降低，连续修复30d，裂缝修复完全，达到优异的修复效果。
实施例3：
（1）称取蔗糖8g、Na2HPO4•12H2O 2g、MgSO4 0.4g、CaCO3 0.5g、KCl 0.1g、(NH4)2SO4 0.4g、酵母提取物0.2g于500mL去离子水中溶解，配置成所需培养基溶液，调节pH为7，125℃高温下灭菌25分钟后取出待冷却，将胶质芽孢杆菌接种至冷却培养基溶液中，30℃下振荡培养，振荡频率为170 r/min，培养时间24h；
（2）将培养好的菌液高速离心10min，离心机转速为8000 rpm，温度为4℃，去除上层培养基营养物质，加去离子水50mL制成浓缩菌液；
（3）取陶粒100g浸泡于50mL胶质芽孢杆菌（Bacillus mucilaginous）浓缩菌液中24h待用，成型水泥基材料水胶比W/C=0.36，胶凝材料用量1300g，称量65g五水乳酸钙与胶凝材料混合均匀，采用内径φ为110mm，高H为45mm的塑料圆柱形试模成型，装模过程将固载有细菌的陶粒集中分布在材料上下表面区域以下5mm范围内；
（4）待试件固化后人工制作裂缝，放入恒温水浴，并持续通入空气养护修复。
修复5d后，裂缝得到较大程度填充，渗透系数大大降低，连续修复30d，可达到优异的修复效果。

Claims (2)

  1. 一种用于修复水泥基材料裂缝的方法，其特征在于，该方法包括以下步骤：
    1）将胶质芽孢杆菌接种至培养基培养中，制备菌体浓度为106~107个/mL的胶质芽孢杆菌浓缩菌液；
    2）将载体浸泡在制备得到的胶质芽孢杆菌浓缩菌液中16~24h，使胶质芽孢杆菌固载于载体中，所述载体为粒径在0.6~0.3mm的陶粒，浓缩菌液和载体的配比为50mL:100g~ 100mL:200g；
    3）把钙源均匀埋入水泥基材料内部，钙源占水泥基材料中胶凝材料的质量百分比为2%~5%，将固载有胶质芽孢杆菌浓缩菌液的载体集中在试件表面区域以下5mm范围内，所述载体占胶凝材料的质量百分比为10%~20%。
  2. 根据权利要求1所述的用于修复水泥基材料裂缝的方法，其特征在于，所述钙源为氯化钙、硝酸钙或乳酸钙。
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