CN102260839A - Method for preparing high-compactness nanometer crystal copper block material - Google Patents
Method for preparing high-compactness nanometer crystal copper block material Download PDFInfo
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- CN102260839A CN102260839A CN 201110203670 CN201110203670A CN102260839A CN 102260839 A CN102260839 A CN 102260839A CN 201110203670 CN201110203670 CN 201110203670 CN 201110203670 A CN201110203670 A CN 201110203670A CN 102260839 A CN102260839 A CN 102260839A
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Abstract
The invention discloses a method for preparing a high-compactness nanometer crystal copper block material, and belongs to the technical field of the preparation of nanometer crystal block materials. In the method, the nanometer crystal copper block material prepared by an inert gas deposition in-situ warm-pressing method is subjected to simple and quick high-current density pulse treatment in an atmospheric environment with high controllability; and the maximum diameter of the prepared nanometer crystal copper block material is 25 millimeters, the maximum thickness is 9.9 millimeters, the average crystallite dimension is between 27 and 45 nanometers, and the compactness is between 99.71 and 99.93 percent. The prepared nanometer crystal copper block material has high heat stability, and grain growth is not obvious at the temperature of below 350 DEG C. The varieties of the nanometer crystal block materials prepared by the method are more, besides the copper material, the method is also suitable for preparing materials such as silver, iron and the like.
Description
Technical field
The present invention relates to the bulk nanometer material preparing technical field, relate in particular to a kind of preparation method of nanocrystalline copper block materials of high-compactness.
Background technology
Bulk nanometer material as a kind of important nano material, has tempting application prospect, is one of focus of nano materials research, and the emphasis of research is the preparation method of bulk nanometer material, microstructure and intrinsic mechanics, corrosive nature etc.The intrinsic performance of research bulk nanometer material, key are to obtain density height, high-quality block materials that microdefect is few.
The preparation method of bulk nanometer material can be divided into two classes substantially, and a class is a two-step approach, promptly prepares nano-crystalline granule earlier, prepares bulk nanometer material by methods such as original position pressurization, hot isostatic pressing, hot extrusion, thermosprays then; Another kind of is single stage method, directly common material is prepared into bulk nanometer material, as amorphous crystallization method, electrodip process, melt solidifying method (comprising High Temperature High Pressure quench method, direct crystallization method and high undercooling crystallization method etc.), intense plastic strain method (comprise high pressure torsion distortion, Equal Channel Angular Pressing, duplex forging, roll over direct sum pressure rolling technology repeatedly etc. repeatedly) etc.In addition, emulsion process, molten slag technology, the Manifold technology that falls, explosion method and dynamic depth plastic deformation method also can be used to prepare bulk nanometer material.Different preparation methods respectively has its advantage and limitation, and for example, high-energy ball milling method technology is simple, and efficient is higher, but easily produces impurity and pollution in the mechanical milling process, is difficult to obtain clean nanocrystal surface; Electrodip process can prepare fine and close bulk nanometer material, but is difficult to prepare the block materials of big thickness.The characteristics of the rare gas element deposition-add in-place platen press in the two-step approach are that nanoparticle has clean Surface, seldom reunite, and the purity height of block, applied widely, be one of bulk nanometer material preparation method of comparative maturity.This kind method constantly is improved in recent years, adopts original position vacuum hotpressing or discharge plasma sintering, can obtain more fine and close nano block, and the microporosity quantity in the block significantly reduces, and the microporosity size reduces greatly.
Lot of domestic and international research institution and colleges and universities have all carried out the preparation and the performance study work of bulk nanometer material, have prepared bulk nano-crystalline copper and have studied mechanical properties such as unit elongation as employing electrodip processes such as the Lu Ke of metal institute of the Chinese Academy of Sciences; The Wang Sheng of metal institute of the Chinese Academy of Sciences has just waited and has utilized severe rolling technology (hot rolling combines with cold rolling and heat treatment phase) to prepare nanocrystalline technically pure iron, 304 stainless steel materials etc., has studied its corrosion behavior in solution such as hydrochloric acid; The Wu Xi person of outstanding talent of Zhejiang University etc. utilizes improved rare gas element deposition-original position temperature and pressure method to prepare block nanometer copper, silver, iron, tungsten etc., and its mechanical property and corrosive nature are studied; The synthetic smelting technologies of employing burning such as the loudspeaker training of Lanzhou chemical physics institute of the Chinese Academy of Sciences is clear have prepared the Fe of diameter 35mm, thickness 7.0mm
3Al matrix body nano material has also been studied mechanical properties such as yield strength.In recent years owing to be subjected to the support of aspect new results such as material, physics and computer modeling technique, about the preparation and the performance study of bulk nanometer material had considerable progress, about the understanding of its strengthening mechanism, toughening mechanism and corrosion behavior also deepens continuously, both at home and abroad the scientific worker is just in unremitting effort, is devoted to the preparation and the intrinsic performance research of density height, high quality nano crystal block body material that microdefect is few.
Copper and alloy thereof are because of its good electrical conductivity, thermal conductivity and good corrosion stability in some medium and good processing characteristics, be important structure, functional and decorative material, be widely used in fields such as electric, light industry, machinofacture, water supply, building, national defence, in the consumption of China's nonferrous materials, be only second to aluminium and alloy thereof.Nanocrystalline copper has huge potential use value because of its nanostructure has special mechanical properties, physicals and chemical property.The nanocrystalline copper block materials of preparation high-compactness not only provides important material foundation for carrying out the research of nanocrystalline copper block materials intrinsic performance, also to the commercial application of nanocrystalline copper, important promoter action is arranged.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of nanocrystalline copper block materials of high-compactness is provided.
The preparation method of the nanocrystalline copper block materials of high-compactness is as follows:
1) adopt purity greater than 99.9% polycrystalline copper block as starting material, put into the crucible in the evaporator room of rare gas element deposition original position temperature and pressure block nanometer material preparation device, evaporator room is evacuated to 4 * 10
-5~ 5 * 10
-5Charge into the high-purity argon gas of 1800 ~ 2000 Pa behind the Pa, with arc plasma with the polycrystalline copper block heating evaporation in the crucible, under the effect of rare gas element convection current, the nanocrystalline copper particle that evaporates is rapid condensation on the liquid nitrogen cold trap outer wall of rotation, every 60 ~ 70 seconds just with the tetrafluoroethylene scraper with the cold-trap outer wall on the nanocrystalline copper particle of condensation scrape to collect and get in the hopper, evaporation powder process finishes then evaporator room and hot pressing chamber to be evacuated to 4 * 10
-5~ 5 * 10
-5Pa, open the vacuum valve between evaporator room and the hot pressing chamber, send in the mould of hot pressing chamber with the nanocrystalline copper powder that mechanical manipulator will be got in the hopper, mould diameter is 25mm, highly is 200 mm, under 200 ℃ of temperature, moulding pressure 1 GPa, insulation 20 minutes, pressurize l hour condition, it is 25mm that nanocrystalline copper powder temperature and pressure are become diameter, and thickness is the nanocrystalline copper block materials of 10mm;
2) nanocrystalline copper block materials upper and lower surface is carried out No. 1000 liquid honings and acetone cleaning after, put it between the last push-down head of high current density burst process device, start high current density burst process device, under 18 ~ 20MPa pressure, the nanocrystalline copper block materials is carried out the high current density burst process, pulse current waveform is the sinusoidal decay ripple, discharge cycle is about 175 μ s, the current amplitude of first pulse is 65000 ~ 70000A, the time length of each burst process is about 700 μ s, the nanocrystalline copper block materials is carried out the high current density burst process 2 ~ 3 times, handling pitch time is 10 minutes, raise seaming chuck after burst process finishes and take out block materials, can obtain the nanocrystalline copper block materials of high-compactness.
The present invention compares with other bulk nanometer material technologies of preparing, mainly has following 4 characteristics:
1) the nanocrystalline copper block materials density height of making is up to 99.93%.
The better heat stability of the nanocrystalline copper block materials of 2) making, not obvious at grain growth below 350 ℃.
3) the nanocrystalline copper block materials to the preparation of rare gas element deposition-original position temperature and pressure method carries out the high current density burst process in atmospheric environment, and simple, convenient, controllability is good.
4) the bulk nanometer material kind that can be made into of the present invention is many, outside the copper removal, also is suitable for materials such as silver, iron.
Description of drawings
Fig. 1 is a homemade large-scale rare gas element deposition-original position temperature and pressure nano material preparation device synoptic diagram of the present invention.
Fig. 2 is a homemade high current density burst process device synoptic diagram of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, describe preparation method in detail according to high-compactness nanocrystalline copper block materials of the present invention.
1) adopt purity greater than 99.9% polycrystalline copper block as starting material, put into the crucible in the evaporator room of homemade large-scale rare gas element deposition original position temperature and pressure block nanometer material preparation device (see figure 1), evaporator room is evacuated to 4 * 10
-5~ 5 * 10
-5Charge into the high-purity argon gas of 1800 ~ 2000 Pa behind the Pa, with arc plasma with the polycrystalline copper block heating evaporation in the crucible, under the effect of rare gas element convection current, the nanocrystalline copper particle that evaporates is rapid condensation on the liquid nitrogen cold trap outer wall of rotation, every 60 ~ 70 seconds minutes just with the tetrafluoroethylene scraper with the cold-trap outer wall on the nanocrystalline copper particle of condensation scrape to collect and get in the hopper.Evaporation powder process finishes the back evaporator room and hot pressing chamber is evacuated to 4 * 10
-5~ 5 * 10
-5Pa, open the vacuum valve between evaporator room and the hot pressing chamber, send in the mould of hot pressing chamber with the nanocrystalline copper powder that mechanical manipulator will be got in the hopper, mould diameter 25mm, height 200 mm, under 200 ℃ of temperature, moulding pressure 1 GPa, insulation 20 minutes, pressurize l hour condition, nanocrystalline copper powder temperature and pressure are become the nanocrystalline copper block materials.
The nanocrystalline copper block materials diameter of rare gas element deposition-original position temperature and pressure method preparation is 25mm, and thickness is 10mm.
2) the nanocrystalline copper block materials upper and lower surface of rare gas element deposition-original position temperature and pressure method preparation is carried out No. 1000 liquid honings and acetone cleaning after, put it between the last push-down head of homemade high current density burst process device (see figure 2), start high current density burst process device, (18 ~ 20MPa) carry out the high current density burst process to the nanocrystalline copper block materials under certain pressure.Pulse current waveform is the sinusoidal decay ripple, and discharge cycle is about 175 μ s, and the current amplitude of first pulse is 65000 ~ 70000A, and the time length of each burst process is about 700 μ s.The amplitude of regulating impulse electric current is selected the nanocrystalline copper block materials of rare gas element deposition-original position temperature and pressure method preparation is carried out the high current density burst process 2 ~ 3 times as required, and handling pitch time is 10 minutes.Raise seaming chuck after burst process finishes and take out block materials, can obtain the nanocrystalline copper block materials of high-compactness.
The maximum diameter of the high-compactness nanocrystalline copper block materials that is obtained is 25mm, and maximum ga(u)ge is 9.9mm, and density is 99.71 ~ 99.93%, and average grain size is 27 ~ 45nm.
Embodiment 1
Adopt purity greater than 99.9% polycrystalline copper block as starting material, put into the crucible in the evaporator room of homemade large-scale rare gas element deposition original position temperature and pressure block nanometer material preparation device, evaporator room is evacuated to 5 * 10
-5Charge into the high-purity argon gas of 1800 Pa behind the Pa, with arc plasma with the polycrystalline copper block heating evaporation in the crucible, under the effect of rare gas element convection current, the nanocrystalline copper particle that evaporates is rapid condensation on the liquid nitrogen cold trap outer wall of rotation, every 70 seconds just with the tetrafluoroethylene scraper with the cold-trap outer wall on the nanocrystalline copper particle of condensation scrape to collect and get in the hopper.Evaporation powder process finishes the back evaporator room and hot pressing chamber is evacuated to 5 * 10
-5Pa, open the vacuum valve between evaporator room and the hot pressing chamber, send in the mould of hot pressing chamber with the nanocrystalline copper powder that mechanical manipulator will be got in the hopper, mould diameter 25mm, height 200 mm, under 200 ℃ of temperature, moulding pressure 1 GPa, insulation 20 minutes, pressurize l hour condition, nanocrystalline copper powder temperature and pressure are become into the nanocrystalline copper block materials of diameter 25mm, thickness 10mm.
After the nanocrystalline copper block materials upper and lower surface of rare gas element deposition-original position temperature and pressure method preparation carried out No. 1000 liquid honings and acetone cleaning, put it between the last push-down head of homemade high current density burst process device, start high current density burst process device, the nanocrystalline copper block materials is carried out the high current density burst process.Processing specification is: pressure 20MPa, and the maximum current amplitude of first pulse is 70000A, 3 high current density burst process, be 10 minutes each pitch time of handling.Raise seaming chuck after burst process finishes and take out block materials, obtain the nanocrystalline copper block materials of the high-compactness of diameter 25mm, thickness 9.9mm.It is 99.71% of theoretical value that Archimedes's method records its density, and it is 27nm that XRD adopts the Scherrer formula to calculate its average grain size.
Embodiment 2
Adopt purity greater than 99.9% polycrystalline copper block as starting material, put into the crucible in the evaporator room of homemade large-scale rare gas element deposition original position temperature and pressure block nanometer material preparation device, evaporator room is evacuated to 4 * 10
-5Charge into the high-purity argon gas of 2000 Pa behind the Pa, with arc plasma with the polycrystalline copper block heating evaporation in the crucible, under the effect of rare gas element convection current, the nanocrystalline copper particle that evaporates is rapid condensation on the liquid nitrogen cold trap outer wall of rotation, every 70 seconds just with the tetrafluoroethylene scraper with the cold-trap outer wall on the nanocrystalline copper particle of condensation scrape to collect and get in the hopper.Evaporation powder process finishes the back evaporator room and hot pressing chamber is evacuated to 5 * 10
-5Pa, open the vacuum valve between evaporator room and the hot pressing chamber, send in the mould of hot pressing chamber with the nanocrystalline copper powder that mechanical manipulator will be got in the hopper, mould diameter 25mm, height 200 mm, under 200 ℃ of temperature, moulding pressure 1 GPa, insulation 20 minutes, pressurize l hour condition, nanocrystalline copper powder temperature and pressure are become into the nanocrystalline copper block materials of diameter 25mm, thickness 10mm.
Diameter 20mm is arrived in the nanocrystalline copper block materials Vehicle Processing of rare gas element deposition-original position temperature and pressure method preparation, after upper and lower surface carried out No. 1000 liquid honings and acetone cleaning, put it between the last push-down head of homemade high current density burst process device, start high current density burst process device, the nanocrystalline copper block materials is carried out the high current density burst process.Processing specification is: pressure 20MPa, and the maximum current amplitude of first pulse is 70000A, 2 high current density burst process, handling pitch time is 10 minutes.Raise seaming chuck after burst process finishes and take out block materials, the acquisition diameter is that 20mm, thickness are the nanocrystalline copper block materials of the high-compactness of 9.85mm.Archimedes's method records 99.93 % that its density is theoretical value, and it is 39nm that XRD adopts the Scherrer formula to calculate its average grain size.
Embodiment 3
Adopt purity greater than 99.9% polycrystalline copper block as starting material, put into the crucible in the evaporator room of homemade large-scale rare gas element deposition original position temperature and pressure block nanometer material preparation device, evaporator room is evacuated to 5 * 10
-5Charge into the high-purity argon gas of 1800 Pa behind the Pa, with arc plasma with the polycrystalline copper block heating evaporation in the crucible, under the effect of rare gas element convection current, the nanocrystalline copper particle that evaporates is rapid condensation on the liquid nitrogen cold trap outer wall of rotation, every 60 seconds just with the tetrafluoroethylene scraper with the cold-trap outer wall on the nanocrystalline copper particle of condensation scrape to collect and get in the hopper.Evaporation powder process finishes the back evaporator room and hot pressing chamber is evacuated to 4 * 10
-5Pa, open the vacuum valve between evaporator room and the hot pressing chamber, send in the mould of hot pressing chamber with the nanocrystalline copper powder that mechanical manipulator will be got in the hopper, mould diameter 25mm, height 200 mm, under 200 ℃ of temperature, moulding pressure 1 GPa, insulation 20 minutes, pressurize l hour condition, nanocrystalline copper powder temperature and pressure are become into the nanocrystalline copper block materials of diameter 25mm, thickness 10mm.
Diameter 20mm is arrived in the nanocrystalline copper block materials Vehicle Processing of rare gas element deposition-original position temperature and pressure method preparation, after upper and lower surface carried out No. 1000 liquid honings and acetone cleaning, put it between the last push-down head of homemade high current density burst process device, start high current density burst process device, the nanocrystalline copper block materials is carried out the high current density burst process.Processing specification is: pressure 18MPa, and the maximum current amplitude of first pulse is 65000A, 3 high current density burst process, handling pitch time is 10 minutes.Raise seaming chuck after burst process finishes and take out block materials, the acquisition diameter is that 20mm, thickness are the nanocrystalline copper block materials of the high-compactness of 9.88mm.Archimedes's method records 99.85 % that its density is theoretical value, and it is 35nm that XRD adopts the Scherrer formula to calculate its average grain size.
Embodiment 4
Adopt purity greater than 99.9% polycrystalline copper block as starting material, put into the crucible in the evaporator room of homemade large-scale rare gas element deposition original position temperature and pressure block nanometer material preparation device, evaporator room is evacuated to 4 * 10
-5Charge into the high-purity argon gas of 2000 Pa behind the Pa, with arc plasma with the polycrystalline copper block heating evaporation in the crucible, under the effect of rare gas element convection current, the nanocrystalline copper particle that evaporates is rapid condensation on the liquid nitrogen cold trap outer wall of rotation, every 60 seconds just with the tetrafluoroethylene scraper with the cold-trap outer wall on the nanocrystalline copper particle of condensation scrape to collect and get in the hopper.Evaporation powder process finishes the back evaporator room and hot pressing chamber is evacuated to 4 * 10
-5Pa, open the vacuum valve between evaporator room and the hot pressing chamber, send in the mould of hot pressing chamber with the nanocrystalline copper powder that mechanical manipulator will be got in the hopper, mould diameter 25mm, height 200 mm, under 200 ℃ of temperature, moulding pressure 1 GPa, insulation 20 minutes, pressurize l hour condition, nanocrystalline copper powder temperature and pressure are become into the nanocrystalline copper block materials of diameter 25mm, thickness 10mm.
Diameter 16mm is arrived in the nanocrystalline copper block materials Vehicle Processing of rare gas element deposition-original position temperature and pressure method preparation, after upper and lower surface carried out No. 1000 liquid honings and acetone cleaning, put it between the last push-down head of homemade high current density burst process device, start high current density burst process device, the nanocrystalline copper block materials is carried out the high current density burst process.Processing specification is: pressure 18MPa, and the maximum current amplitude of first pulse is 70000A, 2 high current density burst process, handling pitch time is 10 minutes.Raise seaming chuck after burst process finishes and take out block materials, the acquisition diameter is that 20mm, thickness are the nanocrystalline copper block materials of the high-compactness of 9.80mm.Archimedes's method records 99.87 % that its density is theoretical value, and it is 45nm that XRD adopts the Scherrer formula to calculate its average grain size.
Claims (1)
1. the preparation method of the nanocrystalline copper block materials of a high-compactness is characterized in that its step is as follows:
1) adopt purity greater than 99.9% polycrystalline copper block as starting material, put into the crucible in the evaporator room of rare gas element deposition original position temperature and pressure block nanometer material preparation device, evaporator room is evacuated to 4 * 10
-5~ 5 * 10
-5Charge into the high-purity argon gas of 1800 ~ 2000 Pa behind the Pa, with arc plasma with the polycrystalline copper block heating evaporation in the crucible, under the effect of rare gas element convection current, the nanocrystalline copper particle that evaporates is rapid condensation on the liquid nitrogen cold trap outer wall of rotation, every 60 ~ 70 seconds just with the tetrafluoroethylene scraper with the cold-trap outer wall on the nanocrystalline copper particle of condensation scrape to collect and get in the hopper, evaporation powder process finishes then evaporator room and hot pressing chamber to be evacuated to 4 * 10
-5~ 5 * 10
-5Pa, open the vacuum valve between evaporator room and the hot pressing chamber, send in the mould of hot pressing chamber with the nanocrystalline copper powder that mechanical manipulator will be got in the hopper, mould diameter is 25mm, highly is 200 mm, under 200 ℃ of temperature, moulding pressure 1 GPa, insulation 20 minutes, pressurize l hour condition, it is 25mm that nanocrystalline copper powder temperature and pressure are become diameter, and thickness is the nanocrystalline copper block materials of 10mm;
2) nanocrystalline copper block materials upper and lower surface is carried out No. 1000 liquid honings and acetone cleaning after, put it between the last push-down head of high current density burst process device, start high current density burst process device, under 18 ~ 20MPa pressure, the nanocrystalline copper block materials is carried out the high current density burst process, pulse current waveform is the sinusoidal decay ripple, discharge cycle is about 175 μ s, the current amplitude of first pulse is 65000 ~ 70000A, the time length of each burst process is about 700 μ s, the nanocrystalline copper block materials is carried out the high current density burst process 2 ~ 3 times, handling pitch time is 10 minutes, raise seaming chuck after burst process finishes and take out block materials, can obtain the nanocrystalline copper block materials of high-compactness.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104690205A (en) * | 2015-01-27 | 2015-06-10 | 浙江大学 | Die and method for preparing large-size three-dimensional full-density nanocrystalline iron body material |
| CN109030542A (en) * | 2017-06-09 | 2018-12-18 | 武汉尚赛光电科技有限公司 | A kind of organic material heat stability testing equipment |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103331449B (en) * | 2013-06-05 | 2015-09-02 | 华南理工大学 | Ultra-fine Grained/micron crystal block body iron material of the two size distribution of a kind of super-high-plasticity and preparation method thereof |
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| CN1401802A (en) * | 2002-04-10 | 2003-03-12 | 昆明理工大学 | Method for mfg. nanograin crystal reinforced copper based material |
| CN101635315A (en) * | 2009-08-18 | 2010-01-27 | 郑直 | Chemical method for preparing three-dimensional dendritic copper selenide nano-crystalline photoelectric film material |
| KR20110032191A (en) * | 2009-09-22 | 2011-03-30 | 영남대학교 산학협력단 | Manufacturing method of nano-grained copper alloys and nano-grained copper alloys obtained thereby |
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| CN1401802A (en) * | 2002-04-10 | 2003-03-12 | 昆明理工大学 | Method for mfg. nanograin crystal reinforced copper based material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104690205A (en) * | 2015-01-27 | 2015-06-10 | 浙江大学 | Die and method for preparing large-size three-dimensional full-density nanocrystalline iron body material |
| CN104690205B (en) * | 2015-01-27 | 2016-08-17 | 浙江大学 | The mould of the three-dimensional large scale full-compact nanometer crystalline substance iron block materials of preparation and method |
| CN109030542A (en) * | 2017-06-09 | 2018-12-18 | 武汉尚赛光电科技有限公司 | A kind of organic material heat stability testing equipment |
| CN109030542B (en) * | 2017-06-09 | 2021-04-09 | 湖北尚赛光电材料有限公司 | Organic material thermal stability test equipment |
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