CN100360613C - A kind of thermosensitive composite material and preparation method thereof - Google Patents
A kind of thermosensitive composite material and preparation method thereof Download PDFInfo
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Abstract
本发明提供了一种温敏复合材料，所述的温敏复合材料由表面包覆有石蜡保护膜的纳米铜粒组成。制备所述的温敏材料的方法如下：将铜粉与石蜡混合后，在惰性气体保护下，用球磨机球磨50～150小时得到所述的温敏复合材料。本发明所述的温敏材料及其制备方法的有益效果主要体现在：(1)所述温敏复合材料热响应速度快、热膨胀性好、且可随意加工成形；(2)原料廉价、普通，工艺简单、成本低，利于工业化生产。The invention provides a temperature-sensitive composite material. The temperature-sensitive composite material is composed of nano-copper particles whose surface is covered with a paraffin protective film. The method for preparing the temperature-sensitive material is as follows: after mixing copper powder and paraffin, under the protection of an inert gas, ball milling with a ball mill for 50-150 hours to obtain the temperature-sensitive composite material. The beneficial effects of the temperature-sensitive material and the preparation method thereof of the present invention are mainly reflected in: (1) the temperature-sensitive composite material has fast thermal response speed, good thermal expansion, and can be processed and formed at will; (2) the raw material is cheap and common , the process is simple, the cost is low, and it is beneficial to industrialized production.
Description
(一)技术领域(1) Technical field
本发明涉及一种温敏复合材料，尤其是一种纳米铜基温敏复合材料。The invention relates to a temperature-sensitive composite material, in particular to a nanometer copper-based temperature-sensitive composite material.
(二)背景技术(2) Background technology
温敏材料集传感、驱动和材料结构于一体，具有感知、驱动和自动控制等功能，是制造高精度温敏测控元件和机构的核心技术之一，也是当今材料科学发展的重要趋势。Temperature-sensitive materials integrate sensing, driving and material structure, and have the functions of perception, driving and automatic control.
目前，国内外对温敏材料的研制主要集中在双金属片、形状记忆合金、温敏形状记忆聚合物和温敏铁氧体等几个领域。对于双金属片和形状记忆合金来说，虽然具有良好的热敏性，但是材料形状固定，不能随测控元件结构而变，做成各种复杂形状的制件，所以具有很大的局限性，并且热双金属片还存在着不稳定性等缺点。在形状记忆合金中，镍钛基合金形状记忆效果好但价格昂贵，铜基合金虽然价格低廉，但记忆性能稳定性差，铁基合金刚开始研究，技术还不成熟。形状记忆聚合物和形状记忆合金相比具有记忆效应大、感应温度低、价廉、易加工成型、适应范围广等特点，近来备受人们的关注，但也尚存在如形变回复力小，回复精度不高，且多为单向记忆等不足之处。温敏铁氧体材料和一般铁氧体不同，它对铁氧体材料本身的物理性能要求高，因此也有很大的局限性。At present, the research and development of temperature-sensitive materials at home and abroad are mainly concentrated in several fields such as bimetallic sheets, shape memory alloys, temperature-sensitive shape memory polymers and temperature-sensitive ferrites. For bimetal sheets and shape memory alloys, although they have good heat sensitivity, the shape of the material is fixed and cannot be changed with the structure of the measurement and control element. There are also disadvantages such as instability in the bimetal sheet. Among shape memory alloys, nickel-titanium-based alloys have good shape memory effect but are expensive. Although copper-based alloys are cheap, they have poor memory performance stability. Iron-based alloys have just begun to be studied, and the technology is not yet mature. Compared with shape memory alloys, shape memory polymers have the characteristics of large memory effect, low induction temperature, low price, easy processing and molding, and wide application range. The accuracy is not high, and most of them are deficiencies such as one-way memory. Different from general ferrite, temperature-sensitive ferrite material has high requirements on the physical properties of ferrite material itself, so it also has great limitations.
(三)发明内容(3) Contents of the invention
为解决现有温敏材料技术中存在的上述不足，本发明提供了一种热敏性好、原料廉价工艺简单、成本低的温敏材料及其制备方法。In order to solve the above-mentioned deficiencies in the existing technology of temperature-sensitive materials, the present invention provides a temperature-sensitive material with good heat sensitivity, cheap raw materials, simple process and low cost and a preparation method thereof.
为达到发明目的本发明采用的技术方案是：For achieving the purpose of the invention, the technical scheme adopted by the present invention is:
一种温敏复合材料，所述的温敏复合材料由表面包覆有石蜡保护膜的纳米铜粒组成，所述石蜡保护膜与纳米铜粒质量之比为5～20∶40。尽管石蜡作为温敏材料具有热膨胀性好的优点，但其作为有机物存在导热系数低的缺点，由于石蜡本身的导热系数很低，导致其热响应速度慢。而铜粉的导热系数很大，因此考虑在石蜡中添加铜粉提高材料的热敏性。A temperature-sensitive composite material. The temperature-sensitive composite material is composed of nano-copper particles coated with a paraffin protective film on the surface, and the mass ratio of the paraffin protective film to the nano-copper particles is 5-20:40. Although paraffin wax has the advantage of good thermal expansion as a temperature-sensitive material, it has the disadvantage of low thermal conductivity as an organic substance. Due to the low thermal conductivity of paraffin wax itself, its thermal response speed is slow. The thermal conductivity of copper powder is very large, so it is considered to add copper powder to paraffin to improve the heat sensitivity of the material.
所述的温敏复合材料质量组成如下：The mass composition of the temperature-sensitive composite material is as follows:
铜粉 40份Copper powder 40 parts
熔点为35～65℃的石蜡 5～20份。5-20 parts of paraffin wax with a melting point of 35-65°C.
进一步，所述的温敏复合材料质量组成如下：Further, the mass composition of the temperature-sensitive composite material is as follows:
铜粉 40份Copper powder 40 parts
熔点为47～51℃的石蜡 5～20份。5-20 parts of paraffin wax with a melting point of 47-51°C.
再进一步，所述的温敏复合材料质量组成如下：Further, the mass composition of the temperature-sensitive composite material is as follows:
铜粉40份，熔点为47～51℃的石蜡5份。40 parts of copper powder, 5 parts of paraffin wax with a melting point of 47-51°C.
制备所述的温敏材料的方法，所述的方法如下：将质量比为40∶5～20的铜粉与石蜡混合后，在惰性气体保护下，用球磨机球磨50～150小时得到所述的温敏复合材料。所述的惰性气体是对铜粉稳定的气体，具体指氦、氖、氩、氪、氙、氮。The method for preparing the temperature-sensitive material is as follows: After mixing copper powder and paraffin wax with a mass ratio of 40:5-20, under the protection of an inert gas, use a ball mill for 50-150 hours to obtain the described Temperature Sensitive Composite Materials. The inert gas is a gas stable to copper powder, specifically helium, neon, argon, krypton, xenon, nitrogen.
进一步，所述的方法如下：将质量为40份的铜粉与5～20份熔点为35～65℃的石蜡混合均匀，在氩气保护下，由高能球磨机球磨50～150小时得到所述的温敏复合材料。Further, the method is as follows: 40 parts by mass of copper powder and 5 to 20 parts of paraffin wax with a melting point of 35 to 65°C are uniformly mixed, and under the protection of argon, ball milling is carried out by a high-energy ball mill for 50 to 150 hours to obtain the described Temperature Sensitive Composite Materials.
由于利用高能球磨法已成功的制备了纳米复合材料、纳米晶纯金属等材料，因此本发明中选择高能法球磨来制备纳米铜基温敏复合材料，使石蜡包覆在纳米铜粒周围，形成了一层保护膜，隔绝了铜粒和空气的接触，提高了铜粒的抗氧化性能，并且由于纳米材料的小尺寸效应，当铜粉达到纳米级后，其导热系数变大，从而提高了整个复合材料的热敏性。Since materials such as nanocomposites and nanocrystalline pure metals have been successfully prepared by high-energy ball milling, high-energy ball milling is selected to prepare nano-copper-based temperature-sensitive composite materials in the present invention, so that paraffin is coated around the nano-copper particles to form A layer of protective film is formed, which isolates the contact between copper particles and air, improves the oxidation resistance of copper particles, and due to the small size effect of nanomaterials, when the copper powder reaches the nanoscale, its thermal conductivity becomes larger, thereby improving Thermal sensitivity of the entire composite.
优选的，所述的方法如下：将质量为40份的铜粉与20份的石蜡(熔点48～51℃)混合均匀，在氩气保护下，由高能球磨机球磨80小时得到所述的温敏复合材料。Preferably, the method is as follows: 40 parts by mass of copper powder and 20 parts of paraffin (melting point 48-51° C.) are evenly mixed, and under the protection of argon, the temperature-sensitive powder is obtained by ball milling in a high-energy ball mill for 80 hours. composite material.
本发明所述的温敏材料及其制备方法的有益效果主要体现在：(1)所述温敏复合材料热响应速度快、热膨胀性好、且可随意加工成形；(2)原料廉价、普通，工艺简单、成本低，利于工业化生产。The beneficial effects of the temperature-sensitive material and the preparation method thereof of the present invention are mainly reflected in: (1) the temperature-sensitive composite material has fast thermal response speed, good thermal expansion, and can be processed and formed at will; (2) the raw material is cheap and common , the process is simple, the cost is low, and it is beneficial to industrialized production.
(四)具体实施方式(4) Specific implementation methods
下面结合具体方式对本发明进行进一步描述：The present invention is further described below in conjunction with specific mode:
实施例1：Example 1:
原料配制：铜粉2kg，石蜡(熔点43～45℃)1kgRaw material preparation: copper powder 2kg, paraffin wax (melting point 43～45℃) 1kg
材料制备：将各组分按一定比例混合后，置于玛瑙罐中，采用大小不等的玛瑙球，在氩气保护下，由行星式高能球磨机球磨80小时制得所述的温敏复合材料。球磨机转速为200r/min。Material preparation: After mixing the components according to a certain ratio, put them in an agate jar, use agate balls of different sizes, and under the protection of argon, mill the temperature-sensitive composite material by a planetary high-energy ball mill for 80 hours. . The rotational speed of the ball mill is 200r/min.
所得的温敏复合材料装入自制铜管(直径5mm，长度20mm，一端封闭)中，利用热压成型工艺制备成型(成型温度为接近于所选石蜡熔点附近)。置于50℃恒温水浴锅，在40秒相对膨胀量达7.5％，复合材料未溶解溃散，伸出部分成柱状。The obtained temperature-sensitive composite material was put into a self-made copper tube (diameter 5mm, length 20mm, one end closed), and prepared by hot pressing molding (the molding temperature was close to the melting point of the selected paraffin wax). Placed in a constant temperature water bath at 50°C, the relative expansion reached 7.5% in 40 seconds, the composite material was not dissolved and collapsed, and the protruding part became columnar.
实施例2：Example 2:
原料配制：铜粉4kg，石蜡(熔点43～45℃)1kgRaw material preparation: copper powder 4kg, paraffin wax (melting point 43～45℃) 1kg
材料制备：将各组分按一定比例混合后，置于玛瑙罐中，采用大小不等的玛瑙球，在氩气保护下，由行星式高能球磨机球磨50小时制得所述的温敏复合材料。球磨机转速为200r/min。Material preparation: After mixing the components according to a certain ratio, put them in an agate jar, use agate balls of different sizes, and under the protection of argon, mill the temperature-sensitive composite material by a planetary high-energy ball mill for 50 hours. . The rotational speed of the ball mill is 200r/min.
实施例3：Example 3:
原料配制：铜粉4kg，石蜡(熔点43～45℃)0.5kgRaw material preparation: copper powder 4kg, paraffin wax (melting point 43～45℃) 0.5kg
材料制备：将各组分按一定比例混合后，置于玛瑙罐中，采用大小不等的玛瑙球，在氩气保护下，由行星式高能球磨机球磨100小时制得所述的温敏复合材料。球磨机转速为200r/min。Material preparation: After mixing the components in a certain proportion, put them in an agate jar, use agate balls of different sizes, and under the protection of argon, mill them for 100 hours with a planetary high-energy ball mill to prepare the temperature-sensitive composite material . The rotational speed of the ball mill is 200r/min.
实施例4：Example 4:
原料配制：铜粉4kg，石蜡(熔点47～51℃)2kgRaw material preparation: copper powder 4kg, paraffin wax (melting point 47～51℃) 2kg
材料制备：将各组分按一定比例混合后，置于玛瑙罐中，采用大小不等的玛瑙球，在氩气保护下，由行星式高能球磨机球磨120小时制得所述的温敏复合材料。球磨机转速为200r/min。Material preparation: After mixing the components in a certain proportion, put them in an agate jar, use agate balls of different sizes, and under the protection of argon, mill them for 120 hours with a planetary high-energy ball mill to prepare the temperature-sensitive composite material . The rotational speed of the ball mill is 200r/min.
实施例5：Example 5:
原料配制：铜粉4kg，石蜡(熔点47～51℃)1kgRaw material preparation: copper powder 4kg, paraffin wax (melting point 47～51℃) 1kg
材料制备：将各组分按一定比例混合后，置于玛瑙罐中，采用大小不等的玛瑙球，在氩气保护下，由行星式高能球磨机球磨150小时制得所述的温敏复合材料。球磨机转速为200r/min。Material preparation: After mixing the components in a certain proportion, put them in an agate jar, use agate balls of different sizes, and under the protection of argon, mill them for 150 hours with a planetary high-energy ball mill to prepare the temperature-sensitive composite material . The rotational speed of the ball mill is 200r/min.
实施例6：Embodiment 6:
原料配制：铜粉4kg，石蜡(熔点45～51℃)0.5kgRaw material preparation: copper powder 4kg, paraffin wax (melting point 45～51℃) 0.5kg
材料制备：将各组分按一定比例混合后，置于玛瑙罐中，采用大小不等的玛瑙球，在氩气保护下，由行星式高能球磨机球磨80小时制得所述的温敏复合材料。球磨机转速为200r/min。Material preparation: After mixing the components according to a certain ratio, put them in an agate jar, use agate balls of different sizes, and under the protection of argon, mill the temperature-sensitive composite material by a planetary high-energy ball mill for 80 hours. . The rotational speed of the ball mill is 200r/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7919646B2 (en) | 2006-07-14 | 2011-04-05 | Invista North America S.A R.L. | Hydrocyanation of 2-pentenenitrile |
| CN101890506B (en) * | 2010-07-31 | 2013-04-24 | 太原理工大学 | Method for preparing nano-copper |
| CN101949004A (en) * | 2010-09-10 | 2011-01-19 | 常州大学 | Preparation method of nano copper film-based copper nano structure |
| CN102303114B (en) * | 2011-05-30 | 2013-06-26 | 深圳市格林美高新技术股份有限公司 | Cladding cobalt powder and preparation method thereof |
| CN102746827B (en) * | 2012-07-04 | 2014-06-04 | 浙江工业大学 | Preparation method for nanometer copper/paraffin thermo-sensitive composite material |
| CN106563802B (en) * | 2015-10-08 | 2020-02-07 | 荆门市格林美新材料有限公司 | Preparation method of granular coated cobalt powder |
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| JPS59216025A (en) * | 1983-05-24 | 1984-12-06 | Teikoku Piston Ring Co Ltd | Wax element type remote temperature detector and transmitter |
| CN1061809A (en) * | 1990-12-01 | 1992-06-10 | 曹松山 | The manufacture method of electroformed copper mould and prescription thereof |
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Assignee: Zhejiang Kangyi Sanitary Ware Co., Ltd. Assignor: Zhejiang University of Technology Contract fulfillment period: 2009.5.10 to 2014.5.10 contract change Contract record no.: 2009330001365 Denomination of invention: Temperature sensitive composite materials and preparing process thereof Granted publication date: 20080109 License type: Exclusive license Record date: 2009.6.9 |
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