CN105821233A - Method for preparing graphene particle reinforced tin lead alloy - Google Patents
Method for preparing graphene particle reinforced tin lead alloy Download PDFInfo
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- CN105821233A CN105821233A CN201610413309.2A CN201610413309A CN105821233A CN 105821233 A CN105821233 A CN 105821233A CN 201610413309 A CN201610413309 A CN 201610413309A CN 105821233 A CN105821233 A CN 105821233A
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- graphene
- powder
- alanine
- lead alloy
- leypewter
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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
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/1005—Pretreatment of the non-metallic additives
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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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- Materials Engineering (AREA)
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Abstract
The invention relates to the field of tin lead alloy materials, in particular to a method for preparing graphene particle reinforced tin lead alloy. The method includes the steps that alanine and graphite powder are mixed to be uniform according to the mass ratio of 1: 1, ball milling is conducted for 24 hours, mixed powder which is mixed to be uniform is obtained, alanine is utilized to strip graphite powder, and grapheme is obtained; grapheme and alanine mixed powder are dispersed in an ethanol solution, and alanine is dissolved; filtering is conducted, and graphene wet powder is obtained; the graphene wet powder is placed in a vacuum drying oven and dried for 18 hours at the temperature of 130 DEG C, and graphene dried powder is prepared, superfine graphite dried powder is blown into tin lead alloy melt through argon, reinforced particles are generated, then mechanical mixing and stirring, modification, refining and pouring are conducted, and the graphene particle reinforced tin lead alloy material is obtained. Wear resistance, strength and performance of the graphene particle reinforced tin lead alloy material are remarkably improved, meanwhile organization stability is good, and electric conduction and heat conduction properties are effectively improved.
Description
Technical field
The present invention relates to a kind of leypewter Material Field, particularly relate to a kind of method preparing Graphene granule reinforced tin metal.
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 a small amount of antimony.The ashbury metal of leaded 38.1% is commonly called as scolding tin, fusing point about 183 DEG C, the welding of element in electrical instrumentation industry, and automobile radiators, heat exchanger, the sealing etc. of Food & Drink container.Leypewter is widely used in the industry, especially as tin-lead solder, by tin-lead solder, various elements is attached molding, but connects the problem that joint portion exists poor mechanical property.Recently as the requirement developing high-end electronic product, requirement to the mechanical property of soldering alloy needs to improve further, granule reinforced tin lead alloy material can play soldering alloy substrate simultaneously and strengthen the advantage of phase, significantly improves the intensity of leypewter, elastic modelling quantity, hardness and wearability.Granule reinforced tin lead alloy material is with low cost because of it simultaneously, and intensity, rigidity are high, the modern industrialization production field such as makes at first system and has wide practical use.
Based on above-mentioned purpose, using and add Graphene granule nontoxic, free of contamination in soldering alloy to strengthen the intensity of soldering alloy material, it is thus achieved that good toughness and hardness, meanwhile, conduction and heat conductivility effectively improve.Chemical composition and the mass fraction of matrix material leypewter of the present invention be: lead Pb:37-42, and residue composition is stannum Sn.The existing leypewter of China is in patent 94120102.3 at present, in order to improve silver and the antimony element of 0.1-5% containing 0.1-5% in the composition of this leypewter of bonding strength.In patent 00115593.8, also it is containing noble metals such as antimony, silver, bismuth, mischmetals, although the toughness of leypewter material, hardness and wearability can be improved, but it is the increase in the melting cost of leypewter, simultaneously, reach higher intensity and wearability, need to further investigate further.The present invention proposes a kind of stable processing technology, low production cost, non-pollution discharge, the preparation method of Graphene granule reinforced tin lead alloy material that can produce in conventional melting condition undertissue, and the more traditional intensity of leypewter material, toughness, hardness and wearability are substantially improved.Therefore, reach to strengthen the purpose of leypewter material mechanical performance in the present invention by adding Graphene granule.
Summary of the invention
It is an object of the invention to: be to overcome above-mentioned prior art not enough, thering is provided a kind of stable processing technology, low production cost, non-pollution discharge, the preparation method of Graphene granule reinforced tin lead alloy material that can produce in conventional melting condition undertissue, the more traditional intensity of leypewter material, toughness, hardness and wearability are substantially improved.
The technical scheme of patent of the present invention is: the present invention is the preparation method of a kind of Graphene granule reinforced tin lead alloy material, by alanine, graphite powder according to quality 1:1 ratio mix homogeneously, the mixed-powder that ball milling is uniformly mixed for 24 hours, in mechanical milling process, utilize alanine to be peeled off by graphite powder and obtain Graphene.Graphene and alanine mixed-powder are scattered in ethanol solution, alanine is dissolved；Filter, obtain Graphene wet-milling；And described Graphene wet-milling is placed in vacuum drying oven in 130 DEG C, dry 18 hours, prepare Graphene dry powder, Graphene dry powder is obtained superfine graphite alkene dry powder in 24 hours through ball milling, by argon, superfine graphite alkene dry powder is blown in leypewter melt, generate and strengthen granule, then through mechanization mix and blend, Metamorphism treatment, refine, cast, i.e. obtain Graphene granule reinforced tin lead alloy material.
Graphene it is scattered in dehydrated alcohol with alanine mixed-powder by above-mentioned preparation method and stirs, after being processed 5 minutes-10 minutes by sonic oscillation, alanine being dissolved, continuing sonic oscillation and process 10 minutes-50 minutes, filter, obtain Graphene wet-milling.
In above-mentioned preparation method, alanine, graphite powder are according to quality 1:1 ratio mix homogeneously, and ball milling obtains the mixed-powder to mix homogeneously in 24 hours, in mechanical milling process, utilize alanine to be peeled off by graphite powder and obtain Graphene.
Gas in above-mentioned preparation method is argon, and the pressure of gas is 0.05-0.3Mpa, gas flow 0.02-0.15m3/Min.Argon is diluent, for reaction speed and particle growth rate.
The temperature of the leypewter melt in above-mentioned preparation method must control below 280 DEG C, prevents Graphene from decomposing in metal bath.
The preparation method of Graphene granule reinforced tin lead alloy material, temperature 180-260 DEG C of leypewter melt.The time of reaction generation enhancing granule is 10-60 minute, and the time that the highest reaction of granule content requirement generates enhancing granule is the longest.
(1) increased response is the Graphene sheet-like particle of synthesis under melt state mutually, fully reacts with leypewter melt and combine under melt state.
The size strengthening granule is 0.1-1 μm.By response time, reaction temperature, the composition etc. of mixed gas are carried out associated adjustment, reaction can be controlled and generate the enhancing composition of granule, particle size, quantity and distribution, thus meet the use requirement of different parts.
The matrix of the present invention uses the chemical composition of alloy and the mass fraction to be: lead Pb:37-42, residue composition is stannum Sn.Can require to carry out melting by mentioned component.In the melting in resistance heating crucible stove of leypewter matrix material, the leypewter material that intensity, toughness and hardness are substantially improved finally can be obtained.
This Graphene granule reinforced tin lead alloy material is without special equipment (without using the equipment such as vacuum melting furnace, High Temperature High Pressure), production can be organized in conventional tin-lead alloy factory, tin metal melt after melting is directly poured in casting mold well prepared in advance, artificial tooth is made after cooling, small investment of the present invention, instant effect, cost of quickly recouping capital outlay.
Compared with existing leypewter technology, the preparation method of Graphene granule reinforced tin lead alloy material has the advantage that
(1) wearability, intensity and property significantly improve, and the poor mechanical property being spaced 2 hours cast samples is less than 6%, and this is beneficial to high-volume, the steady production of small-size materials.Strengthening particle size tiny, be evenly distributed, structure stability is high, and surface no-pollution is well combined with at leypewter matrix.Room-temperature mechanical property and the anti-wear performance of material significantly improve, the application of the aspects such as the element being particularly suitable in electrical instrumentation industry.
(2) structure stability is good, conduction and heat conductivility effectively improve, simultaneously, toxic gas or solute will not be decomposed, the present invention is to be that reaction generates in leypewter melt because strengthening granule, solves additional granule and tin metal matrix wettability is poor, the problem such as interfacial reaction and structure stability difference easily occurs.Particle size because generating is little, and the floating/subsidence velocity caused because of difference in specific gravity is little, is difficult to segregation, and the technology stability of production is high.
Accompanying drawing explanation
It is presented herein below and in conjunction with the accompanying drawings and embodiments specific embodiments of the present invention is described in detail.
Fig. 1 obtains the optics microstructure photo of the sample of Graphene granule reinforced tin lead alloy material；
Fig. 2 obtains the load-deformation curve of the sample of Graphene granule reinforced tin lead alloy material.
Can be seen that the evengranular distribution of Graphene in the sample from the Graphene granule reinforced tin metal optical photograph shown in Fig. 1, the matrix of leypewter comprises uniform Graphene granule, it is possible to be greatly improved mechanical property and the electric conductivity of leypewter.From the Graphene granule reinforced tin metal sample tensile stress-strain curve shown in Fig. 2, it can be seen that intensity relatively conventional specimen improves 25%.
Detailed description of the invention
Highly preferred embodiment of the present invention is given below: according to chemical composition ranges, melting leypewter of the present invention in resistance heating crucible stove.Chemical composition and the mass fraction of leypewter matrix material of the present invention be: lead Pb:37-42, and residue composition is stannum Sn.Treat that it melts and is superheated to 245 DEG C, skim, rotten, refine, running castings；Metal bath is heated to 260 DEG C, with argon, superfine graphite alkene dry powder is blown in leypewter melt, gas pressure 0.1Mpa, gas flow 0.05m3/ Min, 10 minutes time, mixed-powder addition is the 5% of tin metal melt weight, then carries out Metamorphism treatment and refining treatment, running castings, then is incubated, and respectively at 20 points, 80 points of running castings.Then carry out T6 process, and carry out performance test.Test result indicate that Graphene granule reinforced tin lead alloy material tensile strength is 49.15Mpa, Brinell hardness 28, corrosive nature: weightless ratio is 0.01725%, and cost is 3 yuan/Kg.Such as room temperature tensile strength 42.16Mpa after being incubated 80 minutes, Brinell hardness 26, corrosive nature: weightless ratio is 0.01758%, and cost is 3 yuan/Kg.Although the price of Graphene granule reinforced tin lead alloy material of the present invention is slightly above tradition leypewter as can be seen here simultaneously, but the tensile strength of material of the present invention, wearability, especially hardness and structure stability all significantly improve, and stable processing technique is good, it is simple to produce in enormous quantities.
Claims (4)
1. the method preparing Graphene granule reinforced tin metal, it is characterized in that being blown in leypewter melt by superfine graphite alkene dry powder by argon, generate and strengthen granule, then through mechanization mix and blend, Metamorphism treatment, refine, cast, i.e. obtain Graphene granule reinforced tin lead alloy material.
A kind of method preparing Graphene granule reinforced tin metal the most according to claim 1, is characterized in that the chemical composition of matrix material leypewter and mass fraction are: lead Pb:37-42, and residue composition is stannum Sn.
A kind of method preparing Graphene granule reinforced tin metal the most according to claim 1, it is characterized in that Graphene dry powder be by by alanine, graphite powder according to quality 1:1 ratio mix homogeneously, ball milling obtains the mixed-powder to mix homogeneously in 24 hours, in mechanical milling process, utilize alanine to be peeled off by graphite powder and obtain Graphene, Graphene and alanine mixed-powder are scattered in ethanol solution, alanine is dissolved；Filter, obtain Graphene wet-milling；And described Graphene wet-milling is placed in vacuum drying oven in 130 DEG C, dry 18 hours, prepare Graphene dry powder.
A kind of method preparing Graphene granule reinforced tin metal the most according to claim 1, is characterized in that the temperature of leypewter melt must control below 280 DEG C, prevents Graphene from decomposing in metal bath.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610413309.2A CN105821233A (en) | 2016-06-14 | 2016-06-14 | Method for preparing graphene particle reinforced tin lead alloy |
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| CN201610413309.2A CN105821233A (en) | 2016-06-14 | 2016-06-14 | Method for preparing graphene particle reinforced tin lead alloy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107200947A (en) * | 2017-05-22 | 2017-09-26 | 成都新柯力化工科技有限公司 | A kind of graphene microchip conducting masterbatch and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130218A (en) * | 2013-03-25 | 2013-06-05 | 中国科学院上海硅酸盐研究所 | Preparation method of graphene |
| CN105140524A (en) * | 2015-08-28 | 2015-12-09 | 天能电池集团有限公司 | Lead storage battery grid containing lead-graphene composite material |
| US20160012939A1 (en) * | 2014-07-11 | 2016-01-14 | Merry Electronics (Suzhou) Co., Ltd. | Tinsel Wire |
-
2016
- 2016-06-14 CN CN201610413309.2A patent/CN105821233A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130218A (en) * | 2013-03-25 | 2013-06-05 | 中国科学院上海硅酸盐研究所 | Preparation method of graphene |
| US20160012939A1 (en) * | 2014-07-11 | 2016-01-14 | Merry Electronics (Suzhou) Co., Ltd. | Tinsel Wire |
| CN105140524A (en) * | 2015-08-28 | 2015-12-09 | 天能电池集团有限公司 | Lead storage battery grid containing lead-graphene composite material |
Non-Patent Citations (1)
| Title |
|---|
| 杜长华等: "《电子微连接技术与材料》", 29 February 2008, 机械工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107200947A (en) * | 2017-05-22 | 2017-09-26 | 成都新柯力化工科技有限公司 | A kind of graphene microchip conducting masterbatch and preparation method thereof |
| CN107200947B (en) * | 2017-05-22 | 2019-08-20 | 成都新柯力化工科技有限公司 | A kind of graphene microchip conducting masterbatch and preparation method thereof |
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Application publication date: 20160803 |
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