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CN107285748B - Preparation method of ceramic composite material for emulsification pump plunger - Google Patents

Preparation method of ceramic composite material for emulsification pump plunger Download PDF

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CN107285748B
CN107285748B CN201710482374.5A CN201710482374A CN107285748B CN 107285748 B CN107285748 B CN 107285748B CN 201710482374 A CN201710482374 A CN 201710482374A CN 107285748 B CN107285748 B CN 107285748B
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plunger
ceramic
parts
alumina
powder
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CN107285748A (en
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王旭东
杨建锋
王子敬
张亚明
王波
李春芳
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Fugu County Xuli Electromechanical Technology Co ltd
Xian Jiaotong University
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Xian Jiaotong University
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Abstract

一种用于乳化泵柱塞的陶瓷复合材料的制备方法,首先将氧化铝、六方氮化硼、氧化镁、氧化钙、透辉石进行充分混合,再与莫来石晶须进行充分混合后造粒,粉料置于模具中等静压成形,再将其烧结成致密的氧化铝陶瓷柱塞毛坯件,最后通过磨削加工成具有精密尺寸和精度的陶瓷柱塞;与现有技术相比,本发明的陶瓷柱塞材料可以有效地提高陶瓷柱塞的韧性,降低柱塞的摩擦系数,改善材料的磨削加工型和成品率,提高陶瓷柱塞的使用寿命。A method for preparing a ceramic composite material for an emulsification pump plunger. First, alumina, hexagonal boron nitride, magnesium oxide, calcium oxide and diopside are fully mixed, and then fully mixed with mullite whiskers. Granulation, the powder is placed in a mold for isostatic pressing, then sintered into a dense alumina ceramic plunger blank, and finally processed into a ceramic plunger with precise size and precision by grinding; compared with the prior art The ceramic plunger material of the present invention can effectively improve the toughness of the ceramic plunger, reduce the friction coefficient of the plunger, improve the grinding processing type and yield of the material, and increase the service life of the ceramic plunger.

Description

一种用于乳化泵柱塞的陶瓷复合材料的制备方法A kind of preparation method of ceramic composite material for emulsifying pump plunger

技术领域technical field

本发明涉及陶瓷复合材料制备领域,特别涉及一种用于乳化泵柱塞的陶瓷复合材料的制备方法。The invention relates to the field of preparation of ceramic composite materials, in particular to a preparation method of a ceramic composite material for emulsifying pump plungers.

背景技术Background technique

乳化液泵站是综采工作面的关键设备之一,其正常运行直接影响高产高效工作面的生产效益。由于乳化液泵的工作周期较长,故对其关键件陶瓷柱塞的质量要求相当严格。The emulsion pumping station is one of the key equipments in the fully mechanized mining face, and its normal operation directly affects the production efficiency of the high-yield and high-efficiency working face. Due to the long working cycle of the emulsion pump, the quality requirements of its key ceramic plunger are quite strict.

从耐磨性进行比较,氧化锆陶瓷是增韧氧化铝陶瓷的2倍,增韧氧化铝陶瓷是氧化铝陶瓷的4倍以上;从断裂韧性进行比较,氧化锆陶瓷是增韧氧化铝的陶瓷的2-3倍,增韧氧化铝陶瓷是氧化铝陶瓷的2倍左右。氧化锆陶瓷性能最适合煤矿的使用条件,但从经济角度上考虑,氧化锆陶瓷价格昂贵、性价比低,氧化铝陶瓷价格便宜但耐磨性和韧性不够。因此乳化液泵柱塞材料选择增韧氧化铝陶瓷最为合理,并且柱塞在运动过程中可能产生局部瞬时的热量,增韧氧化铝陶瓷比氧化锆在高温下更加稳定。In terms of wear resistance, zirconia ceramics are twice that of toughened alumina ceramics, and toughened alumina ceramics are more than 4 times that of alumina ceramics; in terms of fracture toughness, zirconia ceramics are toughened alumina ceramics. 2-3 times that of toughened alumina ceramics is about 2 times that of alumina ceramics. The performance of zirconia ceramics is most suitable for the conditions of use in coal mines, but from an economic point of view, zirconia ceramics are expensive and cost-effective, while alumina ceramics are cheap but not enough in terms of wear resistance and toughness. Therefore, the selection of toughened alumina ceramics for the plunger material of the emulsion pump is the most reasonable, and the plunger may generate local instantaneous heat during the movement process. The toughened alumina ceramics are more stable at high temperatures than zirconia.

晶须是具有一定长径比(直径0.1-1.8um,长35-150um),且缺陷少的陶瓷单晶。具有很高的强度,是一种非常好的陶瓷基复合材料的增韧增强体;纤维长度较陶瓷晶须长数倍,也是一种很好的陶瓷增韧体,同时两者可复合实用。用SiC、Si3N4等晶须或C、SiC等长纤维对氧化铝陶瓷进行复合增韧。晶须或纤维的加入可以增加断裂表面,即增加了裂纹的扩展通道。当裂纹扩展的剩余能量渗入到纤维(晶须),发生纤维(晶须)的拔出、脱粘和断裂时,导致断裂能被消耗或裂纹扩展方向发生偏转等,从而使复合材料韧性得到提高。但当晶须、纤维含量较高时,由于其拱桥效应而使致密化变得困难,从而引起密度的下降和性能下降。The whiskers are ceramic single crystals with a certain aspect ratio (0.1-1.8um in diameter and 35-150um in length) and few defects. It has high strength and is a very good toughening reinforcement of ceramic matrix composites; the fiber length is several times longer than that of ceramic whiskers, and it is also a good ceramic toughening body, and the two can be combined and practical. Alumina ceramics are composite toughened with whiskers such as SiC and Si3N4 or long fibers such as C and SiC. The addition of whiskers or fibers can increase the fracture surface, that is, increase the crack propagation channel. When the residual energy of crack propagation penetrates into the fibers (whiskers), and the fibers (whiskers) are pulled out, debonded and fractured, the fracture energy is consumed or the direction of crack propagation is deflected, etc., thereby improving the toughness of the composite material. . However, when the whisker and fiber content is high, densification becomes difficult due to its arch bridge effect, resulting in a decrease in density and a decrease in performance.

对于乳化泵陶瓷柱塞来说,柱塞与密封圈之间的滑动摩擦磨损是影响密封的重要因素,而柱塞与密封圈之间的润滑对于降低摩擦系数是重要的手段。For the ceramic plunger of the emulsion pump, the sliding friction and wear between the plunger and the sealing ring is an important factor affecting the sealing, and the lubrication between the plunger and the sealing ring is an important means to reduce the friction coefficient.

发明内容SUMMARY OF THE INVENTION

为了克服上述现有技术的缺点,本发明的目的在于提供一种用于乳化泵柱塞的陶瓷复合材料的制备方法,在原料中添加了可以起到增韧作用的莫来石晶须、起到润滑作用的六方氮化硼以及改善烧结致密性的各种烧结助剂,可以有效提高氧化铝陶瓷柱塞的烧结致密性、材料的韧性和润滑性。In order to overcome the above-mentioned shortcomings of the prior art, the object of the present invention is to provide a method for preparing a ceramic composite material for emulsifying a pump plunger. Hexagonal boron nitride to lubricate and various sintering aids to improve sintering compactness can effectively improve the sintering compactness, toughness and lubricity of alumina ceramic plungers.

为了达到上述目的,本发明采取的技术方案为:In order to achieve the above object, the technical scheme adopted in the present invention is:

一种用于乳化泵柱塞的陶瓷复合材料的制备方法,包括以下步骤:A preparation method of a ceramic composite material for emulsification pump plunger, comprising the following steps:

步骤一;成形粉料的调制:Step 1; Modulation of forming powder:

将氧化铝粉与六方氮化硼、氧化镁、氧化钙、透辉石充分混合后再与莫来石晶须进行充分混合,得到的粉体进行造粒;所述的造粒粉体包括以下组分及重量份数:氧化铝65-90,六方氮化硼2-6,氧化镁1-3,氧化钙1-5,透辉石1-5,莫来石晶须5-20。Alumina powder is fully mixed with hexagonal boron nitride, magnesium oxide, calcium oxide, and diopside, and then fully mixed with mullite whiskers, and the obtained powder is granulated; the granulated powder includes the following Components and parts by weight: alumina 65-90, hexagonal boron nitride 2-6, magnesium oxide 1-3, calcium oxide 1-5, diopside 1-5, mullite whisker 5-20.

步骤二;等静压成型;Step 2; isostatic pressing;

将步骤一中得到的混合物颗粒置于模具中冷等静压成形,成形压力200-500MPa,保压时间1-10min,得到的坯体直接进行粗加工;The mixture particles obtained in step 1 are placed in a mold to form by cold isostatic pressing, the forming pressure is 200-500MPa, and the pressure holding time is 1-10min, and the obtained blank is directly roughened;

步骤三;高温烧结;Step 3; high temperature sintering;

将得到的粗加工的坯体进行高温烧结成致密化铝复合材料坯体,高温烧结温度为1500-1600℃。;The obtained rough-processed body is sintered at high temperature into a densified aluminum composite body, and the high-temperature sintering temperature is 1500-1600°C. ;

步骤四;磨削加工;Step 4; Grinding;

将致密氧化铝复合陶瓷柱塞坯体磨削加工成陶瓷柱塞。The compact alumina composite ceramic plunger body is ground into a ceramic plunger.

所述的步骤二中的模具由耐油橡胶管套、多孔保持架、芯棒和胶塞构成。The mold in the second step is composed of an oil-resistant rubber tube sleeve, a porous cage, a mandrel and a rubber plug.

本发明的有益效果:Beneficial effects of the present invention:

本发明的优点在于,可以有效提高氧化铝陶瓷的致密性和加工效率,改善柱塞的断裂韧性和润滑性,实现制备密度高、韧性好、润滑性优良、尺寸精度高的氧化铝陶瓷柱塞的目的,采用这种致密氧化铝陶瓷柱塞作为柱塞泵的核心部件,具有使用寿命长、耐磨、摩擦系数低的优越性,减少停机维修更换柱塞和密封套的次数,节约工程运行成本,还可以扩展到其他氧化铝部件。The invention has the advantages that the compactness and processing efficiency of the alumina ceramic can be effectively improved, the fracture toughness and lubricity of the plunger can be improved, and the alumina ceramic plunger with high density, good toughness, excellent lubricity and high dimensional accuracy can be prepared. For the purpose of using this kind of dense alumina ceramic plunger as the core component of the plunger pump, it has the advantages of long service life, wear resistance and low friction coefficient, reducing the number of downtimes for repairing and replacing the plunger and sealing sleeve, and saving engineering operation. The cost can also be extended to other alumina components.

同时由于六方氮化硼的添加,有效改善了材料的可加工性,提高了磨削的生产效率。经磨削加工,直径和圆度尺寸公差范围为<0.01mm,表面光洁度为0.2。At the same time, due to the addition of hexagonal boron nitride, the machinability of the material is effectively improved, and the grinding production efficiency is improved. After grinding, the diameter and roundness dimensional tolerance range is <0.01mm, and the surface finish is 0.2.

具体实施方式Detailed ways

下面对本发明进一步说明。The present invention is further described below.

实施例一Example 1

本实施例的制备方法,包括以下步骤:The preparation method of the present embodiment comprises the following steps:

步骤一;成形粉料的调制:Step 1; Modulation of forming powder:

将氧化铝粉与六方氮化硼、氧化镁、氧化钙、透辉石充分混合后再与莫来石晶须进行充分混合,得到的粉体在陶瓷容器中用水做介质充分球磨混合,用喷雾造粒机干燥造粒;按照以下的重量份数配方配制:The alumina powder is fully mixed with hexagonal boron nitride, magnesium oxide, calcium oxide and diopside, and then fully mixed with mullite whiskers. The obtained powder is fully ball-milled and mixed with water as a medium in a ceramic container, and sprayed The granulator is dried and granulated; according to the following formula in parts by weight:

Figure GDA0001400291370000041
Figure GDA0001400291370000041

步骤二;等静压成型;Step 2; isostatic pressing;

将步骤一中得到的混合物颗粒装入由芯棒、耐油橡胶套管、多孔保持架及胶塞构成的专用成型模具,密封后放入冷等静压机的油缸中,在400MPa的压力下保压5分钟成型;脱模后先进行毛坯粗加工;The mixture particles obtained in step 1 were put into a special molding die composed of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, and after sealing, they were put into the oil cylinder of the cold isostatic press, and kept under the pressure of 400MPa. Press for 5 minutes to form; after demoulding, rough machining is performed first;

步骤三;高温烧结;Step 3; high temperature sintering;

将得到的粗加工的坯体进行高温烧结成致密化铝复合材料坯体,在1550度的烧结温度下,保温180分钟;The obtained rough-processed body is sintered at high temperature into a densified aluminum composite body, and the temperature is kept at a sintering temperature of 1550 degrees for 180 minutes;

步骤四;磨削加工;Step 4; Grinding;

将致密氧化铝复合陶瓷柱塞坯体经粗磨和精磨,制成致密氧化铝陶瓷柱塞;相对密度为99.2%,直径公差0.005-0.01mm,表面粗糙度0.2。The dense alumina composite ceramic plunger body is roughly ground and finely ground to make the dense alumina ceramic plunger; the relative density is 99.2%, the diameter tolerance is 0.005-0.01mm, and the surface roughness is 0.2.

实施例二Embodiment 2

本实施例的制备方法,包括以下步骤:The preparation method of the present embodiment comprises the following steps:

步骤一;成形粉料的调制:Step 1; Modulation of forming powder:

将氧化铝粉与六方氮化硼、氧化镁、氧化钙、透辉石充分混合后再与莫来石晶须进行充分混合,得到的粉体在陶瓷容器中用水做介质充分球磨混合,用喷雾造粒机干燥造粒;按照以下的重量份数配方配制:The alumina powder is fully mixed with hexagonal boron nitride, magnesium oxide, calcium oxide and diopside, and then fully mixed with mullite whiskers. The obtained powder is fully ball-milled and mixed with water as a medium in a ceramic container, and sprayed The granulator is dried and granulated; according to the following formula in parts by weight:

Figure GDA0001400291370000051
Figure GDA0001400291370000051

步骤二;等静压成型;Step 2; isostatic pressing;

将步骤一中得到的混合物颗粒装入由芯棒、耐油橡胶套管、多孔保持架及胶塞构成的专用成型模具,密封后放入冷等静压机的油缸中,在350MPa的压力下保压10分钟成型;脱模后先进行毛坯粗加工;The mixture particles obtained in step 1 were put into a special molding die consisting of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber stopper, and after sealing, they were put into the oil cylinder of the cold isostatic press, and kept under the pressure of 350MPa. Press for 10 minutes to form; after demoulding, rough machining is performed first;

步骤三;高温烧结;Step 3; high temperature sintering;

将得到的粗加工的坯体进行高温烧结成致密化铝复合材料坯体,在1530度的烧结温度下,保温180分钟;The obtained rough-machined body is sintered at a high temperature into a densified aluminum composite material body, and the temperature is kept at a sintering temperature of 1530 degrees for 180 minutes;

步骤四;磨削加工;Step 4; Grinding;

将致密氧化铝复合陶瓷柱塞坯体经粗磨和精磨,制成致密氧化铝陶瓷柱塞;相对密度为99.5%,直径公差0.005-0.01mm,表面粗糙度0.2。The dense alumina composite ceramic plunger body is roughly ground and finely ground to make the dense alumina ceramic plunger; the relative density is 99.5%, the diameter tolerance is 0.005-0.01mm, and the surface roughness is 0.2.

实施例三Embodiment 3

本实施例的制备方法,包括以下步骤:The preparation method of the present embodiment comprises the following steps:

步骤一;成形粉料的调制:Step 1; Modulation of forming powder:

将氧化铝粉与六方氮化硼、氧化镁、氧化钙、透辉石充分混合后再与莫来石晶须进行充分混合,得到的粉体在陶瓷容器中用水做介质充分球磨混合,用喷雾造粒机干燥造粒;按照以下的重量份数配方配制:The alumina powder is fully mixed with hexagonal boron nitride, magnesium oxide, calcium oxide and diopside, and then fully mixed with mullite whiskers. The obtained powder is fully ball-milled and mixed with water as a medium in a ceramic container, and sprayed The granulator is dried and granulated; according to the following formula in parts by weight:

Figure GDA0001400291370000061
Figure GDA0001400291370000061

步骤二;等静压成型;Step 2; isostatic pressing;

将步骤一中得到的混合物颗粒装入由芯棒、耐油橡胶套管、多孔保持架及胶塞构成的专用成型模具,密封后放入冷等静压机的油缸中,在200MPa的压力下保压3分钟成型;脱模后先进行毛坯粗加工;The mixture particles obtained in step 1 were loaded into a special molding die composed of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, and after sealing, they were placed in the oil cylinder of a cold isostatic press, and kept under a pressure of 200 MPa. Press for 3 minutes to form; after demoulding, rough machining is performed first;

步骤三;高温烧结;Step 3; high temperature sintering;

将得到的粗加工的坯体进行高温烧结成致密化铝复合材料坯体,在1580度的烧结温度下,保温180分钟;The obtained rough-processed body is sintered at high temperature into a densified aluminum composite material body, and the temperature is kept at a sintering temperature of 1580 degrees for 180 minutes;

步骤四;磨削加工;Step 4; Grinding;

将致密氧化铝复合陶瓷柱塞坯体经粗磨和精磨,制成致密氧化铝陶瓷柱塞;相对密度为98.5%,直径公差0.005-0.01mm,表面粗糙度0.2。The dense alumina composite ceramic plunger body is roughly ground and finely ground to make the dense alumina ceramic plunger; the relative density is 98.5%, the diameter tolerance is 0.005-0.01mm, and the surface roughness is 0.2.

实施例四Embodiment 4

本实施例的制备方法,包括以下步骤:The preparation method of the present embodiment comprises the following steps:

步骤一;成形粉料的调制:Step 1; Modulation of forming powder:

将氧化铝粉与六方氮化硼、氧化镁、氧化钙、透辉石充分混合后再与莫来石晶须进行充分混合,得到的粉体在陶瓷容器中用水做介质充分球磨混合,用喷雾造粒机干燥造粒;按照以下的重量份数配方配制:The alumina powder is fully mixed with hexagonal boron nitride, magnesium oxide, calcium oxide, and diopside, and then fully mixed with mullite whiskers. The obtained powder is fully ball-milled and mixed with water as a medium in a ceramic container. The granulator is dried and granulated; according to the following formula in parts by weight:

Figure GDA0001400291370000071
Figure GDA0001400291370000071

步骤二;等静压成型;Step 2; isostatic pressing;

将步骤一中得到的混合物颗粒装入由芯棒、耐油橡胶套管、多孔保持架及胶塞构成的专用成型模具,密封后放入冷等静压机的油缸中,在300MPa的压力下保压1分钟成型;脱模后先进行毛坯粗加工;The mixture particles obtained in step 1 were put into a special molding die composed of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, and after sealing, they were placed in the oil cylinder of a cold isostatic press, and kept under a pressure of 300MPa. Press for 1 minute to form; after demoulding, rough machining is performed first;

步骤三;高温烧结;Step 3; high temperature sintering;

将得到的粗加工的坯体进行高温烧结成致密化铝复合材料坯体,在1500度的烧结温度下,保温180分钟;The obtained rough-processed body is sintered at high temperature into a densified aluminum composite material body, and the temperature is kept at a sintering temperature of 1500 degrees for 180 minutes;

步骤四;磨削加工;Step 4; Grinding;

将致密氧化铝复合陶瓷柱塞坯体经粗磨和精磨,制成致密氧化铝陶瓷柱塞;相对密度为99.0%,直径公差0.005-0.01mm,表面粗糙度0.2。实施例五The dense alumina composite ceramic plunger body is roughly ground and finely ground to make the dense alumina ceramic plunger; the relative density is 99.0%, the diameter tolerance is 0.005-0.01mm, and the surface roughness is 0.2. Embodiment 5

本实施例的制备方法,包括以下步骤:The preparation method of the present embodiment comprises the following steps:

步骤一;成形粉料的调制:Step 1; Modulation of forming powder:

将氧化铝粉与六方氮化硼、氧化镁、氧化钙、透辉石充分混合后再与莫来石晶须进行充分混合,得到的粉体在陶瓷容器中用水做介质充分球磨混合,用喷雾造粒机干燥造粒;按照以下的重量份数配方配制:The alumina powder is fully mixed with hexagonal boron nitride, magnesium oxide, calcium oxide and diopside, and then fully mixed with mullite whiskers. The obtained powder is fully ball-milled and mixed with water as a medium in a ceramic container, and sprayed The granulator is dried and granulated; according to the following formula in parts by weight:

Figure GDA0001400291370000081
Figure GDA0001400291370000081

步骤二;等静压成型;Step 2; isostatic pressing;

将步骤一中得到的混合物颗粒装入由芯棒、耐油橡胶套管、多孔保持架及胶塞构成的专用成型模具,密封后放入冷等静压机的油缸中,在500MPa的压力下保压8分钟成型;脱模后先进行毛坯粗加工;The mixture particles obtained in step 1 were put into a special molding die composed of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, and after sealing, they were placed in the oil cylinder of a cold isostatic press, and kept under a pressure of 500MPa. Press for 8 minutes to form; after demoulding, rough machining is performed first;

步骤三;高温烧结;Step 3; high temperature sintering;

将得到的粗加工的坯体进行高温烧结成致密化铝复合材料坯体,在1600度的烧结温度下,保温180分钟;The obtained rough-machined body is sintered at high temperature into a densified aluminum composite material body, and the temperature is kept at a sintering temperature of 1600 degrees for 180 minutes;

步骤四;磨削加工;Step 4; Grinding;

将致密氧化铝复合陶瓷柱塞坯体经粗磨和精磨,制成致密氧化铝陶瓷柱塞,经粗磨和精磨,制成致密氧化铝陶瓷柱塞;相对密度为99.3%,直径公差0.005-0.01mm,表面粗糙度0.2。The dense alumina composite ceramic plunger body is roughly ground and finely ground to make a dense alumina ceramic plunger, which is roughly ground and finely ground to make a dense alumina ceramic plunger; the relative density is 99.3%, and the diameter tolerance is 99.3%. 0.005-0.01mm, surface roughness 0.2.

Claims (1)

1. The preparation method of the ceramic composite material for the emulsification pump plunger is characterized by comprising the following steps of:
step one; preparing forming powder:
fully mixing alumina powder, hexagonal boron nitride, magnesium oxide, calcium oxide and diopside, and then fully mixing the mixture with mullite whiskers to obtain powder for granulation; the granulation powder comprises the following components in parts by weight: 65-90 parts of alumina, 2-6 parts of hexagonal boron nitride, 1-3 parts of magnesium oxide, 1-5 parts of calcium oxide, 1-5 parts of diopside and 5-20 parts of mullite whisker;
step two; isostatic pressing;
placing the mixture particles obtained in the step one in a mould for cold isostatic pressing forming, wherein the forming pressure is 200 and 500MPa, and the pressure maintaining time is 1-10min to obtain a blank body;
step three; sintering at high temperature;
sintering the obtained blank at high temperature to obtain a densified aluminum composite blank, wherein the high-temperature sintering temperature is 1500-1600 ℃;
step four; grinding;
and grinding the compact alumina composite ceramic plunger blank to obtain the ceramic plunger.
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