CN107285748A - A preparation method of ceramic composite material for emulsification pump plunger - Google Patents
A preparation method of ceramic composite material for emulsification pump plunger Download PDFInfo
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Abstract
Description
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 ceramic composite materials used for emulsification 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。Emulsion pump station is one of the key equipments in fully mechanized mining face, and its normal operation directly affects the production efficiency of high-yield and high-efficiency working face. Due to the long working cycle of the emulsion pump, the quality requirements for its key component, the 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。From the comparison of wear resistance, zirconia ceramics are twice that of toughened alumina ceramics, and the toughened alumina ceramics are more than 4 times that of alumina ceramics; compared from the perspective of fracture toughness, zirconia ceramics are toughened alumina ceramics 2-3 times that of alumina ceramics, and the toughened alumina ceramics are 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, and alumina ceramics are cheap but not wear-resistant and tough enough. Therefore, the choice 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, and the toughened alumina ceramics are more stable than zirconia at high temperatures.
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。Whiskers are ceramic single crystals with a certain aspect ratio (diameter 0.1-1.8um, length 35-150um) and few defects. With high strength, it is a very good toughening reinforcement of ceramic matrix composite materials; 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. Use SiC, Si3N4 and other whiskers or C, SiC and other long fibers to compound and toughen alumina ceramics. The addition of whiskers or fibers can increase the fracture surface, which increases the crack propagation channel. When the remaining energy of the crack propagation penetrates into the fiber (whisker), when the fiber (whisker) is pulled out, debonded and fractured, the fracture energy is consumed or the crack propagation direction is deflected, etc., so that the toughness of the composite material is improved. . However, when the content of whiskers and fibers is high, densification becomes difficult due to its arch bridge effect, resulting in a decrease in density and 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 emulsification 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Contents 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 shortcoming of the prior art, the object of the present invention is to provide a kind of preparation method of the ceramic composite material that is used for emulsification pump plunger, added the mullite whisker that can play toughening effect in raw material, play The lubricating hexagonal boron nitride and various sintering aids to improve the sintering compactness can effectively improve the sintering compactness, toughness and lubricity of the alumina ceramic plunger.
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 that the present invention takes 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 method for preparing 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。The 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: 65-90 aluminum oxide, 2-6 hexagonal boron nitride, 1-3 magnesium oxide, 1-5 calcium oxide, 1-5 diopside, and 5-20 mullite whiskers.
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 for cold isostatic pressing, the forming pressure is 200-500MPa, and the holding time is 1-10min, and the obtained green body is directly roughed;
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℃。;Sintering the obtained roughly machined green body at a high temperature to form a densified aluminum composite material green body, and the high temperature sintering temperature is 1500-1600°C. ;
步骤四;磨削加工;Step 4: Grinding process;
将致密氧化铝复合陶瓷柱塞坯体磨削加工成陶瓷柱塞。The dense alumina composite ceramic plunger body is ground and processed 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 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 of effectively improving the compactness and processing efficiency of alumina ceramics, improving the fracture toughness and lubricity of the plunger, and realizing the preparation of alumina ceramic plungers with high density, good toughness, excellent lubricity and high dimensional accuracy 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, reduces the number of times of shutdown maintenance and replacement of plunger and seal sleeve, and saves engineering operation 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 production efficiency of grinding is improved. After grinding, the tolerance range of diameter and roundness is <0.01mm, and the surface finish is 0.2.
具体实施方式detailed description
下面对本发明进一步说明。The present invention is further described below.
实施例一Embodiment one
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:Fully mix alumina powder with hexagonal boron nitride, magnesium oxide, calcium oxide, and diopside, and then fully mix with mullite whiskers. The obtained powder is fully ball-milled and mixed with water in a ceramic container, and sprayed Granulator dry granulation; formulate according to the following parts by weight:
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;Put the mixture particles obtained in step 1 into a special forming mold consisting of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, seal it and put it into an oil cylinder of a cold isostatic press, and keep Press for 5 minutes to form; after demoulding, rough rough machining is carried out 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;Sinter the obtained rough-processed green body at high temperature into a densified aluminum composite material green body, and keep it warm for 180 minutes at a sintering temperature of 1550 degrees;
步骤四;磨削加工;Step 4: Grinding process;
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 a 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 two
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:Fully mix alumina powder with hexagonal boron nitride, magnesium oxide, calcium oxide, and diopside, and then fully mix with mullite whiskers. The obtained powder is fully ball-milled and mixed with water in a ceramic container, and sprayed Granulator dry granulation; formulate according to the following parts by weight:
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;Put the mixture particles obtained in step 1 into a special forming mold consisting of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, seal it and put it into an oil cylinder of a cold isostatic press, and keep Press for 10 minutes to form; after demoulding, rough rough machining is carried out 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;Sinter the obtained rough-processed green body at high temperature into a densified aluminum composite material green body, and keep it warm for 180 minutes at a sintering temperature of 1530 degrees;
步骤四;磨削加工;Step 4: Grinding process;
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 produce a 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 three
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:Fully mix alumina powder with hexagonal boron nitride, magnesium oxide, calcium oxide, and diopside, and then fully mix with mullite whiskers. The obtained powder is fully ball-milled and mixed with water in a ceramic container, and sprayed Granulator dry granulation; formulate according to the following parts by weight:
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;Put the mixture particles obtained in step 1 into a special forming mold consisting of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, seal it and put it into an oil cylinder of a cold isostatic press, and keep Press for 3 minutes to form; rough rough machining after demoulding;
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;Sinter the obtained rough-processed green body at high temperature into a densified aluminum composite material green body, and keep it warm for 180 minutes at a sintering temperature of 1580 degrees;
步骤四;磨削加工;Step 4: Grinding process;
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 a 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 four
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:Fully mix alumina powder with hexagonal boron nitride, magnesium oxide, calcium oxide, and diopside, and then fully mix with mullite whiskers. The obtained powder is fully ball-milled and mixed with water in a ceramic container, and sprayed Granulator dry granulation; formulate according to the following parts by weight:
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;Put the mixture particles obtained in step 1 into a special forming mold consisting of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, seal it and put it into an oil cylinder of a cold isostatic press, and keep it Press for 1 minute to form; after demoulding, perform rough machining on the blank;
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;Sinter the obtained rough-processed green body at high temperature into a densified aluminum composite material green body, and keep it warm for 180 minutes at a sintering temperature of 1500 degrees;
步骤四;磨削加工;Step 4: Grinding process;
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 produce a 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 five
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:Fully mix alumina powder with hexagonal boron nitride, magnesium oxide, calcium oxide, and diopside, and then fully mix with mullite whiskers. The obtained powder is fully ball-milled and mixed with water in a ceramic container, and sprayed Granulator dry granulation; formulate according to the following parts by weight:
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;Put the mixture particles obtained in step 1 into a special forming mold consisting of a mandrel, an oil-resistant rubber sleeve, a porous cage and a rubber plug, seal it and put it into an oil cylinder of a cold isostatic press, and keep Press for 8 minutes to form; after demoulding, rough rough machining is carried out 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;Sinter the obtained rough-processed green body at high temperature into a densified aluminum composite material green body, and keep it warm for 180 minutes at a sintering temperature of 1600 degrees;
步骤四;磨削加工;Step 4: Grinding process;
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; after rough grinding and fine grinding, a dense alumina ceramic plunger is made; the relative density is 99.3%, and the diameter tolerance 0.005-0.01mm, surface roughness 0.2.
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