CN115233026A - Preparation method of copper-tin alloy - Google Patents
Preparation method of copper-tin alloy Download PDFInfo
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- CN115233026A CN115233026A CN202210599608.5A CN202210599608A CN115233026A CN 115233026 A CN115233026 A CN 115233026A CN 202210599608 A CN202210599608 A CN 202210599608A CN 115233026 A CN115233026 A CN 115233026A
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- Prior art keywords
- copper
- sodium hydroxide
- tin alloy
- water
- solution
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- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical class [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 129
- 150000001879 copper Chemical class 0.000 claims abstract description 41
- 239000007787 solid Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 25
- 239000012266 salt solution Substances 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 11
- 239000010949 copper Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000009689 gas atomisation Methods 0.000 description 5
- 238000011031 large-scale manufacturing process Methods 0.000 description 5
- 238000004663 powder metallurgy Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 1
- 239000005750 Copper hydroxide Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 229910001956 copper hydroxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- 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
- C22C1/1026—Alloys containing non-metals starting from a solution or a suspension of (a) compound(s) of at least one of the alloy constituents
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/02—Alloys based on copper with tin as the next major constituent
Abstract
The invention provides a preparation method of a copper-tin alloy, which comprises the following steps: preparing a copper salt solution: dissolving soluble copper salt in water to form a copper salt solution, wherein the mass ratio of the soluble copper salt to the water is 1:5-20; preparing a sodium hydroxide solution: dissolving sodium hydroxide in water to form a sodium hydroxide solution, wherein the mass ratio of the sodium hydroxide to the water is 1:2-7; reaction: slowly adding the sodium hydroxide solution into the copper salt solution and keeping stirring, adding anhydrous stannic chloride into the mixed solution after the sodium hydroxide solution is completely added, and continuously stirring for 20-60 minutes; after the reaction is finished, filtering out solids in the mixed solution, washing the solids with water, wherein the mass ratio of the water to the solids is 1:2-6, drying the washed solids for 1-3 hours, and roasting the dried solids for 1-3 hours; and introducing hydrogen into the solid after roasting is finished, keeping heating for 1-3 hours, and cooling to room temperature after heating is finished to obtain the copper-tin alloy powder.
Description
Technical Field
The invention belongs to the technical field of alloy preparation, and particularly relates to a preparation method of a copper-tin alloy.
Background
The copper-tin prealloyed powder currently prepared on the market is prepared by a gas atomization method. Because the atomization method is to atomize liquid copper and tin by using inert gas, the produced powder particles are approximately spherical, but when the spherical copper and tin powder is used for conventional powder metallurgy production, the green strength of the spherical copper and tin powder is not high enough.
Therefore, a preparation method of the copper-tin alloy which has good performance and can be used for large-scale production needs to be researched.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the copper-tin alloy, which has good performance and can be used for large-scale production.
The invention provides a preparation method of a copper-tin alloy, which comprises the following steps:
preparing a copper salt solution: dissolving soluble copper salt in water to form a copper salt solution, wherein the mass ratio of the soluble copper salt to the water is 1:5-20;
preparing a sodium hydroxide solution: dissolving sodium hydroxide in water to form a sodium hydroxide solution, wherein the mass ratio of the sodium hydroxide to the water is 1:2-7;
reaction: slowly adding the sodium hydroxide solution into the copper salt solution and keeping stirring, adding anhydrous stannic chloride into the mixed solution after the sodium hydroxide solution is completely added, and continuously stirring for 20-60 minutes;
after the reaction is finished, filtering out solids in the mixed solution, washing the solids with water, wherein the mass ratio of the water to the solids is 1:2-6, drying the washed solids for 1-3 hours, and roasting the dried solids for 1-3 hours;
and introducing hydrogen into the solid after roasting is finished, keeping heating for 1-3 hours, and cooling to room temperature after heating is finished to obtain the copper-tin alloy powder.
Preferably, in the reaction step, when the sodium hydroxide solution is added to the copper salt solution, the mixed solution is heated to 20-60 ℃ and the stirring speed is 30-400r/min.
Preferably, the soluble copper salt is one of copper chloride, copper sulfate or copper acetate.
Preferably, the mass of the anhydrous tin tetrachloride added is calculated according to the mass ratio of copper to tin of the copper-tin alloy powder to be prepared.
Preferably, the mass ratio of copper to tin of the copper-tin alloy powder is 90: 50.
preferably, the temperature for drying the solid after the reaction is 70-140 ℃.
Preferably, the temperature during calcination is from 140 to 600 ℃.
Preferably, the temperature is heated to 100-350 ℃ during the reaction with the introduction of hydrogen.
Preferably, the molar ratio of soluble copper salt to sodium hydroxide is 2-2.5.
The preparation method of the copper-tin alloy provided by the invention is different from the traditional gas atomization method, and the prepared copper-tin alloy has the following advantages:
1) The finished product of the copper-tin alloy has high purity, small granularity of alloy powder and high microhardness;
2) The copper-tin alloy powder has good fluidity and low apparent density;
3) The copper-tin alloy powder has good plasticity and good wettability, is easy to process, can be used for large-scale production, and can be widely used in the fields of powder metallurgy oil-retaining bearings, diamond tools, filters, powder metallurgy products, bearing bush materials and the like.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular description of preferred embodiments of the invention, as illustrated in the accompanying drawings. Like reference numerals refer to like parts throughout the drawings, and the drawings are not intended to be drawn to scale in actual size, emphasis instead being placed upon illustrating the subject matter.
FIG. 1 is a graph showing the experimental results of the experimental group 1 according to the embodiment of the present invention;
FIG. 2 is a graph showing the results of experiments in Experimental group 2 according to the example of the present invention;
FIG. 3 is a graph showing the results of experiment in Experimental group 3 according to the example of the present invention;
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings.
The technical solutions of the present invention are further described in detail with reference to specific examples so that those skilled in the art can better understand the present invention and can implement the present invention, but the examples are not intended to limit the present invention.
The embodiment of the invention provides a preparation method of a copper-tin alloy, which comprises the following steps:
preparing a copper salt solution: dissolving soluble copper salt in water to form a copper salt solution, wherein the mass ratio of the soluble copper salt to the water is 1:5-20; when preparing the copper salt solution, the soluble copper salt is fully dissolved in water by stirring, and no solid substance is seen in the solution. The mass ratio of the soluble copper salt to water is 1:5, 1, 10, 1.
Preparing a sodium hydroxide solution: the sodium hydroxide is dissolved in water to form a sodium hydroxide solution, and the mass ratio of the sodium hydroxide to the water is 1:2-7. Deionized water is adopted when preparing the copper salt solution and the sodium hydroxide solution, the deionized water refers to the pure water after removing impurities in the form of ions, and the deionized water can ensure that no other ion disturbing reaction is carried out in the production and preparation process, so that the purity of the product can be ensured. In this example, sodium hydroxide acts as a precipitant in the reaction, and a soluble copper salt reacts with the sodium hydroxide to form Cu (OH) 2 And (4) precipitating. In other embodiments, other strong bases, such as potassium hydroxide, etc., may be employed.
Reaction: and slowly adding the sodium hydroxide solution into the copper salt solution, keeping stirring, adding anhydrous stannic chloride into the mixed solution after the sodium hydroxide solution is completely added, and continuously stirring for 20-60 minutes. When the sodium hydroxide is added into the copper salt solution, the adding speed can be controlled by controlling the flow rate of the sodium hydroxide solution, the slow adding is to ensure that the sodium hydroxide can completely react with the copper salt when being added into the copper salt solution, the design can be adapted to different flow rates according to different production equipment and production scales, and the sodium hydroxide can be ensured to completely react with the copper salt. When the sodium hydroxide solution is added, the mixed solution is heated and kept at 20-60 ℃, preferably 40-60 ℃, and the reaction can be accelerated by increasing the temperature; meanwhile, the stirring speed can be set to be 30-400r/min, and the reaction can be promoted by fully stirring.
After the sodium hydroxide solution is completely added, the anhydrous stannic chloride is continuously added into the mixed solution, at the moment, the sodium hydroxide and the copper salt are completely reacted, the anhydrous stannic chloride is added into the mixed solution to be precipitated and reacted with the copper hydroxide, and the anhydrous stannic chloride can generate a large amount of heat when being dissolved in water, so that the reaction can be accelerated.
And after the reaction is finished, filtering out the solid in the mixed solution, washing the solid with water, and filtering by adopting a centrifugal machine during filtering to completely separate out the solid precipitate in the mixed solution. And after filtering out the solid, continuously cleaning the solid by using deionized water, wherein the solid is cleaned to wash out salt solution adhered to the surface of the solid, so that the solid is ensured not to be doped in subsequent treatment. The washing is performed by adding deionized water to the solid, fully stirring, filtering the solid, and repeating the above steps, wherein the washing is performed at least twice in the present embodiment. When cleaning, the mass ratio of water to solid is 1:2-6, the solid needs to be completely immersed by water, and solid powder is obtained after cleaning. Drying the cleaned solid for 1-3 h with hot air at 70-140 deg.C, and calcining the solid for 1-3 h at 140-600 deg.C.
And after roasting is finished, putting the solid in a hydrogen environment for heating reduction, introducing hydrogen into the roasted solid, keeping heating for 1-3 hours, keeping the temperature at 100-350 ℃, and cooling to room temperature after heating is finished to obtain the copper-tin alloy powder.
In this embodiment, the soluble copper salt is one of copper chloride, copper sulfate or copper acetate. The addition amount of the anhydrous stannic chloride is determined according to the amount of the soluble copper salt and the proportion of copper and tin in the finished product, and the mass proportion of copper and tin in the finished product of the copper-tin alloy is 90-50: 50, such as 90: the color of the alloy powder is yellow brown or dark brown within 20 percent of the tin content, and the color of the alloy powder is gray or dark gray when the tin content exceeds 20 percent.
In this embodiment, when the soluble copper salt and the sodium hydroxide solution are prepared, the molar ratio of the soluble copper salt to the sodium hydroxide is 2-2.5, the content of the sodium hydroxide can exceed the reaction ratio, the excessive sodium hydroxide can ensure that the soluble copper salt can be completely reacted, and the excessive sodium hydroxide can be washed away in the subsequent washing operation.
The preparation method of the copper-tin alloy provided by the invention is different from the traditional gas atomization method, and the prepared copper-tin alloy has the characteristics of small granularity, high microhardness, high purity and the like, is good in forming stability and can be used for large-scale production.
To further illustrate the performance of the copper-tin alloy prepared by the copper-tin alloy preparation method of the invention, the following experiments are performed:
TABLE 1 results of the experiment
Experimental group 1 to experimental group 3 the copper-tin alloy was prepared by the preparation method according to the embodiment of the present invention, and the copper-tin alloy was prepared by the comparative group 1 by the conventional gas atomization method, as shown in fig. 1 to fig. 3, the color of the copper-tin alloy prepared in experimental group 1 was tawny, the color of the copper-tin alloy prepared in experimental group 2 was tan, and the color of the copper-tin alloy prepared in experimental group 3 was gray. The table shows that the indexes of the copper-tin alloy powder, such as the grain diameter, the purity, the apparent density and the like of the copper-tin alloy powder prepared by the preparation method of the copper-tin alloy are not changed greatly under the condition of different copper-tin ratios, namely the preparation method of the copper-tin alloy powder has better uniformity for the preparation of the copper-tin alloy with different copper-tin ratios, the copper-tin alloy powder is stable in forming, and the large-scale production can be realized. Compared with the experimental group 1 and the comparative group 1, the copper-tin ratio of the copper-tin alloy powder in the two groups is the same, but the grain diameter of the alloy powder in the experimental group 1 is obviously smaller than that of the alloy powder in the comparative group 1, and the apparent density of the experimental group 1 is obviously lower than that of the comparative group 1, which shows that compared with the copper-tin alloy prepared by the traditional gas atomization method, the copper-tin alloy powder prepared by the preparation method disclosed by the invention has more excellent physical properties, so that the copper-tin alloy powder further has better application effect, and can be widely applied to the fields of powder metallurgy oil-containing bearings, diamond tools, filters, powder metallurgy products, bearing bush materials and the like.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. The preparation method of the copper-tin alloy is characterized by comprising the following steps of:
preparing a copper salt solution: dissolving soluble copper salt in water to form a copper salt solution, wherein the mass ratio of the soluble copper salt to the water is 1:5-20;
preparing a sodium hydroxide solution: dissolving sodium hydroxide in water to form a sodium hydroxide solution, wherein the mass ratio of the sodium hydroxide to the water is 1:2-7;
reaction: slowly adding the sodium hydroxide solution into the copper salt solution, keeping stirring, adding anhydrous stannic chloride into the mixed solution after the sodium hydroxide solution is completely added, and continuously stirring for 20-60 minutes;
after the reaction is finished, filtering out solids in the mixed solution, washing the solids with water, wherein the mass ratio of the water to the solids is 1:2-6, drying the washed solids for 1-3 hours, and roasting the dried solids for 1-3 hours;
and introducing hydrogen into the solid after roasting is finished, keeping heating for 1-3 hours, and cooling to room temperature after heating is finished to obtain the copper-tin alloy powder.
2. The method of claim 1, wherein in the reacting step, the mixed solution is heated to 20 to 60 ℃ at a stirring speed of 30 to 400r/min while the sodium hydroxide solution is added to the copper salt solution.
3. The method of claim 1, wherein the soluble copper salt is one of copper chloride, copper sulfate, or copper acetate.
4. The method for producing a copper-tin alloy according to claim 1, wherein the mass of the anhydrous tin tetrachloride to be added is calculated from the mass ratio of copper to tin of the copper-tin alloy powder to be produced.
5. The method for preparing the copper-tin alloy according to claim 4, wherein the mass ratio of copper to tin of the copper-tin alloy powder is 90: 50.
6. the method for preparing a copper-tin alloy as claimed in claim 1, wherein the temperature of the solid after the reaction is 70 to 140 ℃ when the solid is dried.
7. The method of claim 1, wherein the firing temperature is 140-600 ℃.
8. The method for producing a copper-tin alloy according to claim 1, wherein the temperature is heated to 100 to 350 ℃ during the reaction with hydrogen gas.
9. The method of claim 1, wherein the molar ratio of soluble copper salt to sodium hydroxide is 2-2.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210599608.5A CN115233026B (en) | 2022-05-30 | 2022-05-30 | Preparation method of copper-tin alloy |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210599608.5A CN115233026B (en) | 2022-05-30 | 2022-05-30 | Preparation method of copper-tin alloy |
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| CN115233026A true CN115233026A (en) | 2022-10-25 |
| CN115233026B CN115233026B (en) | 2024-04-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2528601A (en) * | 1946-01-05 | 1950-11-07 | Metal & Thermit Corp | Copper-tin alloy plating |
| JP2006225691A (en) * | 2005-02-15 | 2006-08-31 | Mitsui Mining & Smelting Co Ltd | Tin-coated copper powder and electrically conductive paste using the tin-coated copper powder |
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| CN113579237A (en) * | 2021-07-15 | 2021-11-02 | 江苏萌达新材料科技有限公司 | Preparation method for reducing apparent density of copper-tin alloy powder |
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| US2528601A (en) * | 1946-01-05 | 1950-11-07 | Metal & Thermit Corp | Copper-tin alloy plating |
| JP2006225691A (en) * | 2005-02-15 | 2006-08-31 | Mitsui Mining & Smelting Co Ltd | Tin-coated copper powder and electrically conductive paste using the tin-coated copper powder |
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| CN115233026B (en) | 2024-04-12 |
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