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CN108456006A - The recyclability restorative procedure of Nixing pottery hallrcuts - Google Patents

The recyclability restorative procedure of Nixing pottery hallrcuts Download PDF

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Publication number
CN108456006A
CN108456006A CN201810525280.6A CN201810525280A CN108456006A CN 108456006 A CN108456006 A CN 108456006A CN 201810525280 A CN201810525280 A CN 201810525280A CN 108456006 A CN108456006 A CN 108456006A
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nixing pottery
until
cracks
green body
mixed slurry
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钟恒成
周昌玮
王宁
黄新
闭宗庭
吴彪
吴尚玉
陈玉星
刘展鹏
刘鹏飞
何艳梅
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Beibu Gulf University
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Qinzhou University
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5024Silicates

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The present invention provides the recyclability restorative procedures of Nixing pottery hallrcuts, include the following steps:1) by flyash and SmCl3Grinding, adds water to stir evenly, obtains mixed serum;2) mixed serum is dipped with brush uniformly to smear at Nixing pottery green body slight crack until complete wetting, spontaneously dries;Continue to dip at mixed serum smearing slight crack until complete wetting, natural drying so repeat, until the crack of dry base substrate is filled;3) green body is smoothed out, 15~30min, natural cooling are fired at 1000~1100 DEG C.The present invention at powerful mullite network structure and slight crack by carrying out cross-fixing, to play the role of repairing slight crack, thin but also more mullite network structure intensity is larger not only, can hinder the sliding of crystal boundary, the extension that can prevent crackle, to effectively prevent secondary cracking.

Description

坭兴陶微裂痕的可再生性修复方法Renewable repair method for microcracks in Nixing pottery

技术领域technical field

本发明涉及坭兴陶的制作工艺,具体涉及坭兴陶微裂痕的可再生性修复方法。The invention relates to a manufacturing process of Nixing pottery, in particular to a reproducible repair method for microcracks in Nixing pottery.

背景技术Background technique

坭兴陶的工艺主要包括以下几个步骤:1)制备坯料:坯料选用横穿钦州市区的钦江以东的泥土,俗称东泥(为软质粘土,颜色为黄白色,含微量石英砂,在坭兴陶的生产工艺中起调整可塑性以结合性作用),和钦江以西地域的泥土,俗称西泥(含有少量K2O、NaO、CaO、MgO、Fe203、TiO2、MnO2,是一种含铁量较高的紫泥石,颜色为紫红色,表面层有少量铁质浸染,为硬质粘土,可塑性及结合性较差),按东泥40~60%、西泥40~60%的重量百分比混合,经研磨、脱水等一系列工艺制成坯料;坯料的含水率为24~25%;2)坯体成型:采用可塑法或注浆法将坯料制成各种器型的坯体;3)修整坯体:将坯体修整以达到设计要求;4)干燥:采用风干法对坯体进行干燥,使坯体水分排除;5)绘画雕刻:在坯体上书写作画并进行雕刻;6):坯体干燥;7)烧制坯体:将干燥的坯体装窑烧制,烧制温度控制在1100~1200℃,烧制时间为10h,冷却后出窑;8)抛光打磨:将坯体抛光打磨,即得。The process of Nixing pottery mainly includes the following steps: 1) Preparation of blank: the blank is selected from the soil east of the Qinjiang River across the urban area of Qinzhou City, commonly known as Dongni (soft clay, yellow-white in color, containing a small amount of quartz sand) , which plays the role of adjusting plasticity and combination in the production process of Nixing pottery), and the soil in the area west of the Qinjiang River, commonly known as Ximu (contains a small amount of K 2 O, NaO, CaO, MgO, Fe 2 0 3 , TiO 2 , MnO 2 is a kind of purple mudstone with high iron content, the color is purple red, the surface layer has a small amount of iron dissemination, it is hard clay, and the plasticity and bonding are poor), according to Dongni 40-60%, Mix 40-60% of Xini by weight, and make blanks through a series of processes such as grinding and dehydration; the moisture content of the blanks is 24-25%; Various types of blanks; 3) trimming the blanks: trimming the blanks to meet the design requirements; 4) drying: using the air-drying method to dry the blanks to remove moisture from the blanks; 6) Dry the green body; 7) Firing the green body: put the dried green body in a kiln to fire, the firing temperature is controlled at 1100-1200°C, the firing time is 10 hours, and it is released after cooling. kiln; 8) Polishing and polishing: polishing and polishing the green body to obtain.

坭兴陶的缺陷就是脆性大,坭兴陶由离子键或共价键所组成的多晶结构,这些化学键的原子不像金属键那样排列紧密,有许多孔隙难以引起位错的移动。共价键有方向性,使晶体结构复杂,且具有较高的抗畸变和阻碍位移运动的能力,缺乏能促使材料变形的滑移系统。坭兴陶一旦受到外加负荷,再加上陶瓷工艺很难避免的在材料表面所构成的微缺陷的存在,它们都构成裂纹源,应力就会在这些裂纹的尖端集中。坭兴陶有没有其他可以消耗外来能量的系统,只有以新的自由能予以交换。所谓新的自由能就是裂纹尖端的扩展形成的新的表面所吸收的能量。这样的结果就造成裂纹的快速扩展而表现为所谓的脆性断裂。The defect of Nixing pottery is its high brittleness. Nixing pottery has a polycrystalline structure composed of ionic bonds or covalent bonds. The atoms of these chemical bonds are not as tightly arranged as metal bonds, and there are many pores that are difficult to cause dislocation movement. Covalent bonds are directional, which makes the crystal structure complex, and has a high ability to resist distortion and hinder displacement movement, and lacks a slip system that can promote material deformation. Once Nixing pottery is subjected to an external load, coupled with the existence of micro-defects formed on the surface of the material that are difficult to avoid in ceramic technology, they all constitute crack sources, and stress will concentrate at the tips of these cracks. Does Nixingtao have any other system that can consume external energy, only to exchange it with new free energy. The so-called new free energy is the energy absorbed by the new surface formed by the extension of the crack tip. The result of this is the rapid propagation of cracks that manifest as so-called brittle fractures.

发明内容Contents of the invention

本发明所要解决的技术问题是提供坭兴陶微裂痕的可再生性修复方法,该工艺彻底修复了坯体的裂痕,还能有效杜绝烧成后二次开裂。The technical problem to be solved by the present invention is to provide a reproducible method for repairing the microcracks of Nixing pottery. This process completely repairs the cracks of the green body and can effectively prevent secondary cracks after firing.

为解决上述技术问题,本发明采用的技术方案是坭兴陶微裂痕的可再生性修复方法,包括以下步骤:In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is a reproducible repair method for Nixing pottery micro-cracks, comprising the following steps:

1)将粉煤灰和SmCl3研磨,加水搅拌均匀,得到混合浆液;1) Grinding the fly ash and SmCl3 , adding water and stirring evenly to obtain a mixed slurry;

2)用刷子蘸取混合浆液均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取混合浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;2) Use a brush to dip the mixed slurry and evenly apply the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the mixed slurry to apply the cracks until it is completely wet, and then dry naturally, and repeat until the cracks of the green body are dry until it is filled;

3)抹平坯体,在1000~1100℃下烧制15~30min,自然冷却。3) Smooth the green body, fire at 1000-1100°C for 15-30 minutes, and cool naturally.

粉煤灰中Al2O3、Fe2O3、MgO为低共熔氧化物,在1000~1100℃下可以形成液相,促进了莫来石的合成,Cl-的存在能降低液相的粘度,液相中的原子更加容易扩散,此条件下莫来石析出的初期具有高的形核率,容易进行的原子扩散加快了棒状晶粒的生长,因此形成了更多的莫来石棒状晶粒。Sm3+能细化棒状莫来石晶粒尺寸,颗粒连接紧密,颗粒间的有效迁移面积和接触面积增大,这些又多又细的莫来石棒状晶粒形成巨大的网络结构,渗入到裂痕深处,与裂痕形成交叉网络,从而起到修复裂痕的作用。又由于又细又多的莫来石网络结构强度较大,能阻碍晶界的滑移,可以防止裂纹的扩展,从而有效防止二次开裂。Al 2 O 3 , Fe 2 O 3 , and MgO in fly ash are eutectic oxides, which can form a liquid phase at 1000-1100 ° C, which promotes the synthesis of mullite. The presence of Cl - can reduce the liquid phase. Viscosity, the atoms in the liquid phase are easier to diffuse. Under this condition, the initial stage of mullite precipitation has a high nucleation rate, and the easy atomic diffusion accelerates the growth of rod-shaped grains, so more mullite rods are formed. grain. Sm 3+ can refine the rod-shaped mullite grain size, the particles are closely connected, and the effective migration area and contact area between particles are increased. These many and fine mullite rod-shaped grains form a huge network structure and penetrate into the Deep in the crack, it forms a cross network with the crack, thus playing the role of repairing the crack. And because the fine and numerous mullite network structure is strong, it can hinder the slippage of the grain boundary, prevent the expansion of cracks, and thus effectively prevent secondary cracking.

稀土氧化物虽然也能起到细化晶粒的作用,但是并不能增加晶粒的数量,晶粒细但是少,也不能起到很好的修复效果,十分容易产生二次开裂。Although the rare earth oxide can also play a role in refining the grains, it cannot increase the number of grains. The grains are fine but few, and cannot play a good repair effect, and it is very easy to cause secondary cracking.

粉煤灰中的低共共熔氧化物在烧结冷却阶段残余液相填充于棒状莫来石晶粒间空隙而起到粘接作用,避免了莫来石生长所导致的结构疏松,进一步提高了修复效果。The eutectic oxide in fly ash fills the gaps between the rod-shaped mullite grains during the sintering and cooling stage to play a bonding role, avoiding the loose structure caused by the growth of mullite, and further improving the Repair effect.

混合浆液的含水率为30~50%。The water content of the mixed slurry is 30-50%.

将粉煤灰研磨至200~400目。Grind the fly ash to 200-400 mesh.

SmCl3的重量为粉煤灰的0.01~0.05%。The weight of SmCl 3 is 0.01-0.05% of the fly ash.

在1000~1050℃下烧制15~20min。Fire at 1000-1050°C for 15-20 minutes.

与现有技术相比,本发明通过强大的莫来石网络结构与裂痕处进行交叉固定,从而起到修复裂痕的作用,又细又多的莫来石网络结构强度较大,能阻碍晶界的滑移,可以防止裂纹的扩展,从而有效防止二次开裂。Compared with the prior art, the present invention cross-fixes the cracks through the strong mullite network structure, thereby repairing the cracks, and the thin and numerous mullite network structure has a higher strength, which can hinder the grain boundary The slippage can prevent the expansion of cracks, thus effectively preventing secondary cracking.

具体实施方式Detailed ways

以下用实施例来进一步说明本发明的实质性内容,但并不以此限定本发明。The following examples are used to further illustrate the substantive content of the present invention, but the present invention is not limited thereto.

以下实验所用坭兴陶坯体均为相同尺寸、相同工艺、相同配方同一批次制作而成的坭兴陶器皿,采用相同的方式进行裂纹处理,裂纹尺寸也一样(长度为3cm,深度为0.5mm)。The Nixing pottery bodies used in the following experiments are all Nixing pottery vessels made in the same batch with the same size, the same process, and the same formula. mm).

实施例1Example 1

1)将粉煤灰和SmCl3研磨至200目,加水搅拌均匀,得到含水率为30%的混合浆液;SmCl3的重量为粉煤灰的0.01%;1) Grind fly ash and SmCl3 to 200 mesh, add water and stir evenly to obtain a mixed slurry with a water content of 30%; the weight of SmCl3 is 0.01% of fly ash;

2)用刷子蘸取混合浆液均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取混合浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;2) Use a brush to dip the mixed slurry and evenly apply the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the mixed slurry to apply the cracks until it is completely wet, and then dry naturally, and repeat until the cracks of the green body are dry until it is filled;

3)抹平坯体,在1000℃下烧制15min,自然冷却。3) Smooth the green body, fire at 1000°C for 15 minutes, and cool naturally.

对裂痕修复处进行抗折强度测试,其强度为104MPa。The flexural strength test was carried out on the crack repaired part, and its strength was 104MPa.

对照例1Comparative example 1

1)将粉煤灰和Sm2O3研磨至200目,加水搅拌均匀,得到含水率为30%的混合浆液;Sm2O3的重量为粉煤灰的0.01%;1) Grind the fly ash and Sm2O3 to 200 mesh, add water and stir evenly to obtain a mixed slurry with a water content of 30%; the weight of Sm2O3 is 0.01% of the flyash;

2)用刷子蘸取混合浆液均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取混合浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;2) Use a brush to dip the mixed slurry and evenly apply the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the mixed slurry to apply the cracks until it is completely wet, and then dry naturally, and repeat until the cracks of the green body are dry until it is filled;

3)抹平坯体,在1000℃下烧制15min,自然冷却。3) Smooth the green body, fire at 1000°C for 15 minutes, and cool naturally.

对裂痕修复处进行抗折强度测试,其强度为49MPa。The flexural strength test was carried out on the crack repaired part, and its strength was 49MPa.

对照例2Comparative example 2

1)将粉煤灰研磨至200目,加水搅拌均匀,得到含水率为30%的混合浆液;1) Grinding the fly ash to 200 mesh, adding water and stirring evenly to obtain a mixed slurry with a moisture content of 30%;

2)用刷子蘸取混合浆液均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取混合浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;2) Use a brush to dip the mixed slurry and evenly apply the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the mixed slurry to apply the cracks until it is completely wet, and then dry naturally, and repeat until the cracks of the green body are dry until it is filled;

3)抹平坯体,在1000℃下烧制15min,自然冷却。3) Smooth the green body, fire at 1000°C for 15 minutes, and cool naturally.

对裂痕修复处进行抗折强度测试,其强度为31MPa。The flexural strength test was carried out on the crack repaired part, and its strength was 31MPa.

对照例3Comparative example 3

1)用刷子蘸取坭兴陶坯料浆液(含水率为30%)均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;1) Use a brush to dip the Nixing pottery blank slurry (moisture content is 30%) and evenly apply it to the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the slurry and apply the slurry until it is completely wet, and then dry naturally Repeat this until the cracks in the dry body are filled;

3)抹平坯体,在1000℃下烧制15min,自然冷却。3) Smooth the green body, fire at 1000°C for 15 minutes, and cool naturally.

对裂痕修复处进行抗折强度测试,其强度为15MPa。The flexural strength test is carried out on the crack repair part, and its strength is 15MPa.

实施例2Example 2

1)将粉煤灰和SmCl3研磨至400目,加水搅拌均匀,得到含水率为50%的混合浆液;SmCl3的重量为粉煤灰的0.05%;1) Grind fly ash and SmCl3 to 400 mesh, add water and stir evenly to obtain a mixed slurry with a water content of 50%; the weight of SmCl3 is 0.05% of fly ash;

2)用刷子蘸取混合浆液均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取混合浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;2) Use a brush to dip the mixed slurry and evenly apply the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the mixed slurry to apply the cracks until it is completely wet, and then dry naturally, and repeat until the cracks of the green body are dry until it is filled;

3)抹平坯体,在1100℃下烧制30min,自然冷却。3) Smooth the green body, fire at 1100°C for 30 minutes, and cool naturally.

对裂痕修复处进行抗折强度测试,其强度为99MPa。The flexural strength test was carried out on the crack repaired part, and its strength was 99MPa.

实施例3Example 3

1)将粉煤灰和SmCl3研磨至300目,加水搅拌均匀,得到含水率为40%的混合浆液;SmCl3的重量为粉煤灰的0.03%;1) Grind fly ash and SmCl3 to 300 mesh, add water and stir evenly to obtain a mixed slurry with a water content of 40%; the weight of SmCl3 is 0.03% of fly ash;

2)用刷子蘸取混合浆液均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取混合浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;2) Use a brush to dip the mixed slurry and evenly apply the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the mixed slurry to apply the cracks until it is completely wet, and then dry naturally, and repeat until the cracks of the green body are dry until it is filled;

3)抹平坯体,在1020℃下烧制18min,自然冷却。3) Smooth the green body, fire at 1020°C for 18 minutes, and cool naturally.

对裂痕修复处进行抗折强度测试,其强度为110MPa。The flexural strength test was carried out on the crack repaired part, and its strength was 110MPa.

实施例4Example 4

1)将粉煤灰和SmCl3研磨至2000目,加水搅拌均匀,得到含水率为50%的混合浆液;SmCl3的重量为粉煤灰的0.01%;1) Grind fly ash and SmCl3 to 2000 mesh, add water and stir evenly to obtain a mixed slurry with a water content of 50%; the weight of SmCl3 is 0.01% of fly ash;

2)用刷子蘸取混合浆液均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取混合浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;2) Use a brush to dip the mixed slurry and evenly apply the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the mixed slurry to apply the cracks until it is completely wet, and then dry naturally, and repeat until the cracks of the green body are dry until it is filled;

3)抹平坯体,在1100℃下烧制15min,自然冷却。3) Smooth the green body, fire at 1100°C for 15 minutes, and cool naturally.

对裂痕修复处进行抗折强度测试,其强度为96MPa。The flexural strength test was carried out on the crack repaired part, and its strength was 96MPa.

Claims (5)

1.坭兴陶微裂痕的可再生性修复方法,其特征在于:包括以下步骤:1. The regenerative repairing method of Nixing pottery microcrack, is characterized in that: comprise the following steps: 1)将粉煤灰和SmCl3研磨,加水搅拌均匀,得到混合浆液;1) Grinding the fly ash and SmCl3 , adding water and stirring evenly to obtain a mixed slurry; 2)用刷子蘸取混合浆液均匀涂抹坭兴陶坯体裂痕处直至完全润湿,自然干燥;继续蘸取混合浆液涂抹裂痕处直至完全润湿,自然干燥,如此重复,直至干燥坯体的裂缝被填满为止;2) Use a brush to dip the mixed slurry and evenly apply the cracks of the Nixing pottery body until it is completely wet, and then dry naturally; continue to dip the mixed slurry to apply the cracks until it is completely wet, and then dry naturally, and repeat until the cracks of the green body are dry until it is filled; 3)抹平坯体,在1000~1100℃下烧制15~30min,自然冷却。3) Smooth the green body, fire at 1000-1100°C for 15-30 minutes, and cool naturally. 2.根据权利要求1所述的坭兴陶微裂痕的可再生性修复方法,其特征在于:混合浆液的含水率为30~50%。2. The reproducible method for repairing microcracks in Nixing pottery according to claim 1, characterized in that the water content of the mixed slurry is 30-50%. 3.根据权利要求1所述的坭兴陶微裂痕的可再生性修复方法,其特征在于:将粉煤灰研磨至200~400目。3. The reproducible repair method for microcracks in Nixing pottery according to claim 1, characterized in that: the fly ash is ground to 200-400 mesh. 4.根据权利要求1所述的坭兴陶微裂痕的可再生性修复方法,其特征在于:SmCl3的重量为粉煤灰的0.01~0.05%。4. The reproducible method for repairing microcracks in Nixing pottery according to claim 1, characterized in that: the weight of SmCl3 is 0.01-0.05% of the fly ash. 5.根据权利要求4所述的坭兴陶微裂痕的可再生性修复方法,其特征在于:在1000~1050℃下烧制15~20min。5. The reproducible method for repairing microcracks in Nixing pottery according to claim 4, characterized in that: firing at 1000-1050° C. for 15-20 minutes.
CN201810525280.6A 2018-05-28 2018-05-28 The recyclability restorative procedure of Nixing pottery hallrcuts Pending CN108456006A (en)

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