CN106011515B - A kind of method for preparing carbon nanotube powder enhancing leypewter - Google Patents
A kind of method for preparing carbon nanotube powder enhancing leypewter Download PDFInfo
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- CN106011515B CN106011515B CN201610439129.1A CN201610439129A CN106011515B CN 106011515 B CN106011515 B CN 106011515B CN 201610439129 A CN201610439129 A CN 201610439129A CN 106011515 B CN106011515 B CN 106011515B
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- leypewter
- carbon nanotube
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
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Abstract
The present invention relates to a kind of leypewter Material Field, more particularly to a kind of method for preparing carbon nanotube powder enhancing leypewter.By preparing following calcium metal Ca, magnesium Mg, copper Cu, aluminium Al, nickel and cobalt and water H2O nitrate solution, its composition proportion are 1：1：1：1：1：1：11.Above-mentioned nitrate solution, nitric acid and sodium hydrate aqueous solution are mixed, by quality 1：1：1 ratio is well mixed, sediment is subjected to filtering acquisition, it is subsequently placed in vacuum drying chamber in 550 DEG C, calcining 18 hours, then the superfines that ball milling is 20 μm in ball mill is catalysts, powder prepared by the above method is placed in steel reactor, volume ratio is blown into steel reactor as 9:1 propylene and the mixed gas of nitrogen, the pressure of body is 0.05 0.3Mpa, and gas flow is 0.4 m3/ Min, reaction temperature are 660 DEG C, and the reaction time is 60 Min, and CNT dry powder is made.Wearability, intensity and the property of carbon nanotube powder enhancing leypewter material significantly improve, while structure stability is good, and conductive and heat conductivility effectively improves.
Description
Technical field
The present invention relates to a kind of leypewter Material Field, and carbon nanotube powder enhancing tin-lead is prepared more particularly to one kind
The method of alloy.
Background technology
One important use of leypewter is to be used as tin-lead solder, and based on leypewter, some tin solders are also containing few
The antimony of amount.Leaded 38.1% tin alloy is commonly called as scolding tin, about 183 DEG C of fusing point, for the welding of element in electrical instrumentation industry, with
And sealing of automobile radiators, heat exchanger, food and beverage container etc..Leypewter has obtained widely should in the industry
With especially as tin-lead solder, various elements being attached with shaping by tin-lead solder, but connect joint portion and power be present
The problem of learning poor performance.Recently as the requirement for developing high-end electronic product, the requirement to the mechanical property of soldering alloy needs
Further to improve, powder enhancing leypewter material can play soldering alloy substrate simultaneously with strengthening the advantage of phase, significantly
Improve intensity, modulus of elasticity, hardness and the wearability of leypewter.Powder strengthens leypewter material because its cost is low simultaneously
Honest and clean, intensity, rigidity are high, formerly enter the modern industrial process fields such as manufacture and have wide practical use.
Based on above-mentioned purpose, strengthen soldering using nontoxic, free of contamination carbon nanotube powder is added in soldering alloy
The intensity of alloy material, good toughness and hardness are obtained, meanwhile, conductive and heat conductivility effectively improves.Base of the present invention
The chemical composition of body material leypewter is：Lead Pb：37-42, remaining composition are tin Sn.The existing leypewter in China exists at present
It is silver-colored and 0.1-5% containing 0.1-5% in the composition of the bonding strength leypewter in order to improve in patent 94120102.3
Antimony element.In patent 00115593.8, and containing noble metals such as antimony, silver, bismuth, mischmetals, although tin-lead conjunction can be improved
Toughness, hardness and the wearability of golden material, but the melting cost of leypewter is the increase in, meanwhile, to reach higher intensity
With wearability, it is necessary to further be furtherd investigate.The present invention proposes a kind of stable processing technology, low production cost, nothing
Disposal of pollutants, the preparation method that leypewter material can be strengthened in the carbon nanotube powder that conventional melting condition undertissue produces,
Intensity, toughness, hardness and the wearability of more traditional leypewter material are substantially improved.Therefore, addition is passed through in the present invention
Carbon nanotube powder reaches the purpose of enhancing leypewter material mechanical performance.
The content of the invention
The purpose of the present invention is：It is to overcome above-mentioned prior art deficiency, there is provided a kind of stable processing technology, production cost
Cheap, non-pollution discharge, the system that leypewter material can be strengthened in the carbon nanotube powder that conventional melting condition undertissue produces
Preparation Method, intensity, toughness, hardness and the wearability of more traditional leypewter material are substantially improved.
The technical scheme of patent of the present invention is：The present invention is a kind of preparation of carbon nanotube powder enhancing leypewter material
Method, prepares the nitrate solution of following calcium metal Ca, magnesium Mg, copper Cu, aluminium Al, nickel and cobalt and water H2O, and its composition proportion is equal
For 1：1：1：1：1：1：11.Above-mentioned nitrate solution, nitric acid and sodium hydrate aqueous solution are mixed, by quality 1：1：1 ratio is mixed
Close uniformly, sediment is subjected to filtering acquisition, is subsequently placed in vacuum drying chamber in 550 DEG C, calcine 18 hours, then in ball milling
Ball milling is that 20 μm of superfines is catalysts in machine, powder prepared by the above method is placed in steel reactor, Xiang Gang
Volume ratio is blown into reactor as 9:1 propylene and the mixed gas of nitrogen, the pressure of body are 0.05-0.3Mpa, gas flow
For 0.4 m3/ Min, reaction temperature are 660 DEG C, and the reaction time is 60 Min, and CNT dry powder is made, dry powder is passed through into ball milling
Ultra-fine CNT dry powder is obtained within 24 hours, ultra-fine CNT dry powder is blown into leypewter melt by argon gas, is generated
Strengthen powder, then by mechanization mixing, Metamorphism treatment, refining, cast, that is, obtain carbon nanotube powder enhancing tin-lead and close
Golden material.
The nitrate solution of calcium metal Ca, magnesium Mg, copper Cu, aluminium Al, nickel and cobalt and water H2O in above-mentioned preparation method, its
Composition proportion is 1：1：1：1：1：1：11.
Nitrate solution, nitric acid and sodium hydrate aqueous solution are according to quality 1 in above-mentioned preparation method：1：The mixing of 1 ratio is equal
It is even, sediment is subjected to filtering acquisition, is subsequently placed in vacuum drying chamber in 550 DEG C, is calcined 18 hours, then in ball mill
The superfines that ball milling is 20 μm is catalysts.
Gas in above-mentioned preparation method is 9：The mixture of 1 propylene and nitrogen, the pressure of gas is 0.05-0.3Mpa,
Gas flow 0.4m3/Min.Nitrogen is diluent, for reaction speed and the powder speed of growth.
The temperature of leypewter melt in above-mentioned preparation method must be controlled below 280 DEG C, prevent CNT from existing
Decomposed in metal bath.
Carbon nanotube powder strengthens the preparation method of leypewter material, 180-260 DEG C of the temperature of leypewter melt.Instead
The time that enhancing powder should be generated is 10-60 minutes, and content of powder requires that the time of higher reaction generation enhancing powder is longer.
（1）Increased response is mutually the CNT flakelike powder synthesized under melt state, is closed under melt state with tin-lead
Golden melt fully reacts and combined.
The size for strengthening powder is 0.1-1 μm.By being carried out to the composition etc. of reaction time, reaction temperature, mixed gas
Associated adjustment, composition, powder size, quantity and the distribution of reaction generation enhancing powder can be controlled, so as to meet different parts
Requirement.
The present invention matrix be using the chemical composition of alloy：Lead Pb：37-42, remaining composition are tin Sn.Can be by upper
State component requirements and carry out melting.In the melting in resistance heating crucible furnace of leypewter matrix material, intensity, tough can be finally obtained
The leypewter material that property and hardness are substantially improved.
The carbon nanotube powder strengthens leypewter material without special equipment（Need not be high using vacuum melting furnace, high temperature
The equipment such as pressure）, can organize to produce in conventional tin-lead alloy factory, the tin metal melt after melting directly be poured into well prepared in advance
Casting mold in, artificial tooth is made after cooling, small investment of the present invention is quick, and can quickly recoup capital outlay cost.
Compared with existing leypewter technology, the preparation method of carbon nanotube powder enhancing leypewter material is with as follows
Advantage：
（1）Wearability, intensity and property significantly improve, and the poor mechanical property for being spaced 2 hours cast samples is less than 6%, and this will have
Beneficial to high-volume, the steady production of small-size materials.It is tiny to strengthen powder size, is evenly distributed, structure stability is high, surface without
Pollution, with being well combined in leypewter matrix.The room-temperature mechanical property and anti-wear performance of material significantly improve, and are particularly suitable for
The application of element in electrical instrumentation industry etc..
（2）Structure stability is good, and conductive and heat conductivility effectively improves, meanwhile, toxic gas or molten will not be decomposed
Thing is solved, the present invention is being that generation is reacted in leypewter melt because strengthening powder to be, solves additional powder and tin metal base
Body wetability is poor, the problems such as interfacial reaction and structure stability difference easily occurs.Because the powder size of generation is small, because difference in specific gravity is led
Floating/subsidence velocity of cause is small, is not easy to be segregated, and the technology stability of production is high.
Brief description of the drawings
Here is that specific embodiments of the present invention are described in detail in conjunction with the accompanying drawings and embodiments.
Fig. 1 obtains the optics microstructure photo of the sample of carbon nanotube powder enhancing leypewter material；
Fig. 2 obtains the load-deformation curve of the sample of carbon nanotube powder enhancing leypewter material.
It can be seen that carbon nanotube powder is uniform from the carbon nanotube powder enhancing leypewter optical photograph shown in Fig. 1
Distribution in the sample, uniform carbon nanotube powder is included in the matrix of leypewter, can greatly improve leypewter
Mechanical property and electric conductivity.It is bent from carbon nanotube powder enhancing leypewter sample tensile stress-strain shown in Fig. 2
Line, it can be seen that intensity improves 41.1% compared with conventional specimen.
Embodiment
Highly preferred embodiment of the present invention is given below：According to chemical composition ranges, the melting sheet in resistance heating crucible furnace
Invention leypewter.The chemical composition of leypewter matrix material of the present invention is：Lead Pb：37-42, remaining composition are tin Sn.Treat
It melts and is superheated to 245 DEG C, skims, go bad, refining, running castings；Metal bath is heated to 260 DEG C, will be super with argon gas
Thin CNT dry powder is blown into leypewter melt, gas pressure 0.1Mpa, the m of gas flow 0.053/ Min, time 10 divide
Clock, mixed-powder addition is the 5% of tin metal melt weight, then carries out Metamorphism treatment and refining treatment, running castings, then is protected
Temperature, and respectively at 20 points, 80 points of running castings.Then T6 processing is carried out, and carries out performance test.Test result indicates that carbon nanometer
Pipe powder enhancing leypewter Tensile strength is 55.41Mpa, Brinell hardness 30, corrosive nature：Weightless ratio is
0.01699%, cost is 3 yuan/Kg.The Mpa of room temperature tensile strength 52.15, Brinell hardness 28, corrosivity after being such as incubated 80 minutes
Energy：Weightless ratio is 0.01711%, and cost is 3 yuan/Kg.Carbon nanotube powder of the present invention strengthens leypewter simultaneously as can be seen here
Although the slightly above traditional leypewter of the price of material, the tensile strength of material of the present invention, especially wearability, hardness and group
Knit stability all to significantly improve, and stable processing technique is good, is easy to produce in enormous quantities.
Claims (3)
- A kind of 1. method for preparing carbon nanotube powder enhancing leypewter, it is characterized in that being done ultra-fine CNT by argon gas Powder is blown into leypewter melt, generation enhancing particle, then by mechanization mixing, Metamorphism treatment, refining, cast, i.e., Obtain carbon nanotube powder enhancing leypewter material；CNT dry powder is by preparing following calcium metal Ca, magnesium Mg, copper Cu, aluminium Al, nickel and cobalt and water H2O nitrate solution, its composition proportion are 1:1：1:1:1:1:11, by above-mentioned nitrate Solution, nitric acid and sodium hydrate aqueous solution mixing, by quality 1:1:1 ratio is well mixed, and sediment is carried out into filtering acquisition, so After be placed in vacuum drying chamber in 550 DEG C, calcine 18 hours, the superfines that then ball milling is 20 μm in ball mill is reaction Catalyst, powder prepared by the above method is placed in steel reactor, volume ratio is blown into steel reactor as 9:1 propylene and The mixed gas of nitrogen, the pressure of gas is 0.05-0.3MPa, and gas flow is 0.4 m3/ min, reaction temperature are 660 DEG C, Reaction time is 60 min, and CNT dry powder is made.
- A kind of 2. method for preparing carbon nanotube powder enhancing leypewter according to claim 1, it is characterized in that matrix The chemical composition and mass fraction of material leypewter be：Lead Pb：37-42, residual components are tin Sn.
- A kind of 3. method for preparing carbon nanotube powder enhancing leypewter according to claim 1, it is characterized in that tin-lead The temperature of alloy melt must be controlled below 280 DEG C, prevent CNT from being decomposed in metal bath.
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| CN101158001A (en) * | 2007-11-23 | 2008-04-09 | 苏州有色金属研究院有限公司 | Vacuum stirring composite granule reinforcing aluminium-based composite material and preparation technique thereof |
| CN104263995A (en) * | 2014-10-09 | 2015-01-07 | 戴国水 | Titanium-based alloy wire |
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| US20070145097A1 (en) * | 2005-12-20 | 2007-06-28 | Intel Corporation | Carbon nanotubes solder composite for high performance interconnect |
| CN101555575B (en) * | 2009-05-07 | 2011-07-06 | 山东交通学院 | Titanium-aluminum intermetallic compound-carbon nano tube compound material preparation method and products |
| CN112355513A (en) * | 2011-08-02 | 2021-02-12 | 阿尔法组装解决方案公司 | Solder composition |
| CN102513720B (en) * | 2011-12-23 | 2014-05-07 | 哈尔滨工业大学深圳研究生院 | High-performance tin-based solder alloy and preparation method thereof |
| CN103628005B (en) * | 2013-11-22 | 2016-03-02 | 江苏大学 | A kind of brake flange carbon fiber reinforced aluminum matrix composite and preparation method |
| KR101654523B1 (en) * | 2014-08-29 | 2016-09-07 | 한국기계연구원 | Hybrid Composite Solder Alloys and Their Fabrication Methods |
| CN105039877B (en) * | 2015-08-05 | 2016-11-30 | 同济大学 | Carbon fiber reinforced aluminum matrix composite and preparation method and application |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101158001A (en) * | 2007-11-23 | 2008-04-09 | 苏州有色金属研究院有限公司 | Vacuum stirring composite granule reinforcing aluminium-based composite material and preparation technique thereof |
| CN104263995A (en) * | 2014-10-09 | 2015-01-07 | 戴国水 | Titanium-based alloy wire |
Non-Patent Citations (1)
| Title |
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| Influence of single-wall carbon nanotube addition on the microstructural and tensile properties of Sn–Pb solder alloy;K. Mohan Kumar et al.;《Journal of Alloys and Compounds》;20081231;第455卷;摘要，第149页左栏第2段，第2.1节 * |
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