CN116262952A - Preparation method of free-cutting porous copper-zinc binary alloy for seal - Google Patents
Preparation method of free-cutting porous copper-zinc binary alloy for seal Download PDFInfo
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- CN116262952A CN116262952A CN202211641523.5A CN202211641523A CN116262952A CN 116262952 A CN116262952 A CN 116262952A CN 202211641523 A CN202211641523 A CN 202211641523A CN 116262952 A CN116262952 A CN 116262952A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
- C22C9/04—Alloys based on copper with zinc as the next major constituent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method of free-cutting porous copper-zinc binary alloy for a seal, which comprises the following steps: (1) drying copper zinc alloy powder and pressing the dried copper zinc alloy powder into a pressed compact; (2) Carrying out reduction treatment on the obtained pressed compact in a reducing atmosphere; (3) Sintering the reduced pressed compact in a protective atmosphere to obtain a sintered body with a pore structure; (4) And (3) performing pore spheroidization on the sintered body in a protective atmosphere, wherein the temperature of the pore spheroidization is 450-600 ℃. The invention prepares the undoped and free-cutting porous copper-zinc binary alloy material through the reduction-sintering-pore spheroidizing integrated process, the process has high production efficiency, low production cost, environmental protection and no pollution, and the seal carved by the material not only can leak stamp pad ink, has high working efficiency and light weight, but also has complete and bright graphics and clear printing text.
Description
Technical Field
The invention relates to the technical field of alloy material preparation, in particular to a preparation method of a free-cutting porous copper-zinc binary alloy for a seal.
Background
Brass has the characteristics of high strength, high hardness, wear resistance, corrosion resistance, good machining performance, long service life and the like, and becomes the preferable material for official seal and fire-lacquer seal. However, brass stamps are heavy and inefficient compared to ink-return stamps, photosensitive stamps, limiting their development and impairing their competitiveness in the stamp market.
The porous metal has good permeability due to the unique pore structure, and the metal printing head is processed by the porous brass material, so that the quality of the seal is reduced, raw materials are saved, and meanwhile, the working efficiency of the seal is improved due to the seepage seal oil structure similar to that of the photosensitive seal. However, because of the existence of the pore structure, firstly, the hardness of brass is low, secondly, the vibration phenomenon occurs in the processing process due to the large rigidity difference of a base body and pores during cutting and uneven stress of a blade, the high-quality processing surface is difficult to cut, the roughness of the processing surface is large, and further, the problems of pattern defect, pits, unclear printing text and the like of a stamp engraved by adopting porous brass are caused.
Machinability of dense brass is generally improved by doping elements such as carbon, silicon, phosphorus, aluminum, magnesium, lead, bismuth, antimony, etc. However, in the case of porous brass, the machinability is affected by both material and porosity. The doping element not only can complicate the preparation process and increase the production cost, but also can pollute the environment if the doping of lead element, and meanwhile, the doping element has less influence on the pore structure; it is therefore difficult to improve machinability of porous brass by doping elements.
Disclosure of Invention
The invention provides a preparation method of a free-cutting porous copper-zinc binary alloy material for a seal, which is used for overcoming the problems of pattern defect, pits, unclear seal marks and the like of the carved seal caused by low hardness and poor cutting performance of porous brass in the prior art, and the free-doping and free-cutting porous copper-zinc binary alloy material is prepared by a reduction-sintering-pore spheroidizing integrated process.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of free-cutting porous copper-zinc binary alloy for seals comprises the following steps:
(1) Drying the copper-zinc alloy powder and pressing the dried copper-zinc alloy powder into a pressed compact;
(2) Carrying out reduction treatment on the obtained pressed compact in a reducing atmosphere;
(3) Sintering the reduced pressed compact in a protective atmosphere at 650-800 ℃ to obtain a sintered body with a pore structure;
(4) And (3) performing pore spheroidization on the sintered body in a protective atmosphere, wherein the temperature of pore spheroidization is 450-600 ℃, and obtaining the free-cutting porous copper-zinc binary alloy for the seal.
According to the invention, the copper-zinc alloy powder is pressed into loose pressed blanks, the sinterability of the copper-zinc alloy powder is improved through reduction treatment, and meanwhile, the residual stress of the pressed blanks in the pressing process is removed, so that deformation and cracks are avoided in the sintering process; then sintering is carried out at a temperature lower than the melting point of the alloy, powder particles are not completely melted, and sintering necks are formed among the particles, so that a sintered body with a pore structure is obtained; finally, through spheroidizing, the atoms in the powder particles diffuse and migrate to the bonding surfaces among the particles, so that the sintering neck is promoted to grow up, the pore diameter is reduced and homogenized, the pore shape is gradually changed from an irregular sheet shape to a spherical shape, and the hardness of the material is improved while the porosity is not influenced. In the invention, the spheroidizing temperature plays a key role: the temperature is too high, although pores are spheroidized, the sintering neck is obviously large, so that the pore diameter is sharply reduced, even the pores are closed, and the porosity is reduced; the temperature is too low, the atomic diffusion migration energy is small, the change of a sintering neck is not obvious, and the pore spheroidization is not ideal.
After the porous copper-zinc alloy pore is spheroidized, the impact force of the cutter on the contact spherical pore defect is smaller than that on the contact irregular pore defect in the cutting process, and meanwhile, the spheroidized pore cuts the continuity of a matrix in the cutting process, so that stress is concentrated, the shearing strength of a local area of the chip is larger than the breaking strength, the chip is broken in a broken state, high-speed cutting is realized, a smooth surface is obtained, and the cutting performance of brass is improved.
The free-cutting porous copper-zinc binary alloy material is prepared by adopting the reduction-sintering-pore spheroidization integrated process, so that pore spheroidization can be promoted, the hardness and cutting processability of the material are improved, and meanwhile, the influence on the porosity and pore diameter is small, and the leakage stamp pad ink capability of the porous copper-zinc alloy is not weakened. The process flow is simple, the production efficiency is high, the copper-zinc alloy components are not required to be changed, the resources are saved, the environment is protected, and the green manufacturing is realized. The seal engraved by the material not only can leak stamp-pad ink, has high working efficiency and light weight, but also has complete and bright image and text and clear stamp-pad text.
Preferably, the copper-zinc alloy powder in the step (1) has a mass ratio of copper to zinc of 1.25 to 1.63, and the particle size of the copper-zinc alloy powder is 40 to 150 μm.
More preferably, the copper-zinc alloy powder has a copper-zinc mass ratio of 1.42 to 1.57.
Preferably, in the step (1), low-temperature vacuum drying is adopted, the drying temperature is 50-80 ℃ and the vacuum degree is 10 -3 ～10 -5 Pa, and drying time is 5-15 h.
Preferably, in the step (1), a limit pressing mode is adopted, the height compression ratio is 1.5-2.5, and the pressure maintaining time is 3-10 s. The invention adopts a limiting pressing mode to press the pressed compact, thereby avoiding errors caused by pressure fluctuation of the hydraulic press.
More preferably, the high compression ratio is 1.7 to 2.3.
Preferably, the reducing atmosphere in the step (2) is hydrogen, and the dew point of the reducing atmosphere is lower than 0 ℃; the temperature during the reduction treatment is 250-450 ℃, the temperature rising rate is 1-5 ℃/min, and the heat preservation time is 0.5-5 h. Because the specific surface area of the raw material powder is large, oxidation is easy to occur, in the reduction process, the sample is not thoroughly reduced due to high dew point of the reduction atmosphere, and the surface of the particles is provided with oxide skin, so that the sample is not thoroughly burned in the subsequent sintering process, the sample strength is low, and layering phenomenon occurs. Therefore, the dew point of the reducing atmosphere in the reduction stage is lower than that in the sintering and spheroidizing stages.
Preferably, the protective atmosphere in the step (3) is selected from one of hydrogen, nitrogen and argon; the temperature rising rate during sintering is 1-10 ℃/min, the heat preservation time is 1-3 h, and the temperature is reduced along with the furnace.
Preferably, the sintered body obtained in the step (3) has a porosity of 5 to 30% and a pore size of 5 to 50. Mu.m. The porosity and pore diameter of the sintered body are in the range, so that the carved seal has good ink leakage capacity.
Preferably, the protective atmosphere in the step (4) is selected from one of hydrogen, nitrogen and argon; the heat preservation time of pore spheroidization is 0.5-3 h, and the pore spheroidization is cooled along with a furnace.
Therefore, the invention has the following beneficial effects:
(1) The free-cutting porous copper-zinc binary alloy material is prepared by adopting a reduction-sintering-pore spheroidizing integrated process, so that pore spheroidization can be promoted, the hardness and cutting processability of the material are improved, meanwhile, the influence on the porosity and pore diameter is small, and the leakage stamp pad ink capability of the porous copper-zinc alloy is not weakened;
(2) The process flow is simple, the production efficiency is high, the copper-zinc alloy components are not required to be changed, the resources are saved, the environment is protected, and the green manufacturing is realized;
(3) The seal engraved by the material not only can leak stamp-pad ink, has high working efficiency and light weight, but also has complete and bright image and text and clear stamp-pad text.
Drawings
Fig. 1 is an SEM morphology of the copper zinc alloy powder used in example 1.
FIG. 2 is a graph showing the reduction-sintering-pore spheroidization process for preparing the porous copper-zinc binary alloy of example 1.
Fig. 3 is a cross-sectional SEM topography of the porous copper zinc binary alloy of comparative example 1.
Fig. 4 is a cross-sectional SEM topography of the porous copper zinc binary alloy of example 1.
FIG. 5 is a graph of the microscopic Vickers hardness comparison of the porous copper-zinc binary alloys of example 1 and comparative example 1.
Fig. 6 is a graph comparing machined surface roughness of porous copper zinc binary alloys in example 1 and comparative example 1.
Fig. 7 is a machined chip morphology graph of the porous copper zinc binary alloy of comparative example 1.
Fig. 8 is a machined chip morphology plot of the porous copper zinc binary alloy of example 1.
Detailed Description
The invention is further described below with reference to the drawings and detailed description.
In the present invention, all raw materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
a preparation method of free-cutting porous copper-zinc binary alloy for seals comprises the following steps:
(1) Placing copper-zinc alloy powder with grain size of 60-75 micrometers and copper-zinc mass ratio of 1.5 in vacuum degree of 10 -5 Carrying out drying treatment at 75 ℃ in a drying oven of Pa, and preserving heat for 10 hours, wherein the morphology of the copper-zinc alloy powder is shown in figure 1;
(2) Placing the dried copper-zinc alloy powder into a die, and pressing by a hydraulic press in a limit pressing mode to form a loose round pressed compact, wherein the height compression ratio is 1.8, and the pressure maintaining time is 3s;
the obtained compact is then subjected to reduction-sintering-pore spheroidization integrated treatment, the process curve is shown in fig. 2, and the treatment method is as follows: (3) Placing the obtained pressed compact in a tube furnace, introducing ammonia with a dew point of-40 ℃ to decompose hydrogen, heating to 300 ℃ at a heating rate of 3 ℃/min, preserving heat for 2.5h, and carrying out reduction treatment;
(4) After the step (3) is finished, continuing to introduce ammonia with the dew point of-15 ℃ for decomposing hydrogen, heating to 650 ℃ at the heating rate of 10 ℃/min, and sintering for 2 hours to obtain a sintered body with a pore structure;
(5) And (3) continuing to introduce ammonia with the dew point of-15 ℃ to decompose hydrogen after the step (4) is completed, cooling to 475 ℃ along with a furnace, preserving heat for 1h, and performing pore spheroidization on the sintered body to obtain the free-cutting porous copper-zinc binary alloy for the seal.
Example 2:
a preparation method of free-cutting porous copper-zinc binary alloy for seals comprises the following steps:
(1) Placing copper-zinc alloy powder with grain size of 60-75 micrometers and copper-zinc mass ratio of 1.5 in vacuum degree of 10 -5 Carrying out drying treatment at 75 ℃ in a drying oven of Pa, and preserving heat for 10 hours, wherein the morphology of the copper-zinc alloy powder is shown in figure 1;
(2) Placing the dried copper-zinc alloy powder into a die, and pressing by a hydraulic press in a limit pressing mode to form a loose round pressed compact, wherein the height compression ratio is 1.9, and the pressure maintaining time is 3s;
(3) Placing the obtained pressed compact in a tube furnace, introducing ammonia with a dew point of-45 ℃ to decompose hydrogen, heating to 350 ℃ at a heating rate of 3 ℃/min, preserving heat for 4 hours, and carrying out reduction treatment;
(4) After the step (3) is finished, continuing to introduce ammonia with the dew point of-20 ℃ for decomposing hydrogen, heating to 700 ℃ at the heating rate of 10 ℃/min, and sintering for 2.5 hours to obtain a sintered body with a pore structure;
(5) And (3) continuing to introduce ammonia with the dew point of-20 ℃ to decompose hydrogen after the step (4) is completed, cooling to 500 ℃ along with a furnace, preserving heat for 2 hours, and performing pore spheroidization on the sintered body to obtain the free-cutting porous copper-zinc binary alloy for the seal.
Example 3:
a preparation method of free-cutting porous copper-zinc binary alloy for seals comprises the following steps:
(1) Placing copper-zinc alloy powder with grain size of 60-75 micrometers and copper-zinc mass ratio of 1.5 in vacuum degree of 10 -5 Carrying out drying treatment at 75 ℃ in a drying oven of Pa, and preserving heat for 10 hours, wherein the morphology of the copper-zinc alloy powder is shown in figure 1;
(2) Placing the dried copper-zinc alloy powder into a die, and pressing by a hydraulic press in a limit pressing mode to form a loose round pressed compact, wherein the height compression ratio is 2.0, and the pressure maintaining time is 3s;
(3) Placing the obtained pressed compact in a tube furnace, introducing ammonia with a dew point of-35 ℃ to decompose hydrogen, heating to 350 ℃ at a heating rate of 3 ℃/min, preserving heat for 2.5h, and carrying out reduction treatment;
(4) After the step (3) is finished, continuing to introduce ammonia with the dew point of-25 ℃ for decomposing hydrogen, heating to 725 ℃ at the heating rate of 10 ℃/min, and sintering for 2 hours to obtain a sintered body with a pore structure;
(5) And (3) continuing to introduce ammonia with the dew point of minus 25 ℃ to decompose hydrogen after the step (4) is completed, cooling to 525 ℃ along with a furnace, preserving heat for 2.5h, and performing pore spheroidization on the sintered body to obtain the free-cutting porous copper-zinc binary alloy for the seal.
Comparative example 1:
comparative example 1 differs from example 1 in that the reduced compact in comparative example 1 was sintered without performing the pore spheroidization of step (5), and the remainder was the same as in example 1.
Comparative example 2 (spheroidizing temperature too low):
comparative example 2 differs from example 1 in that the pore spheroidization temperature of step (5) in comparative example 2 was 350 ℃, and the rest was the same as in example 1.
Comparative example 3 (spheroidizing temperature too high):
comparative example 3 differs from example 1 in that the pore spheroidization temperature of step (5) in comparative example 3 was 700 ℃, and the rest was the same as in example 1.
The porous copper-zinc binary alloys prepared in the above example 1 and comparative example 1 were tested for pore structure, mechanical properties and cutting properties, and the results are shown in fig. 3 to 8 and table 1.
Wherein:
1. open porosity: the open porosity was tested by the vacuum impregnation method according to the test standard of GB/T5164-1985 determination of the open porosity of permeable sintered Metal Material:
wherein:
epsilon is the percent open cell content in percent by volume;
m 1 the weight of the non-oiled (dried) sample in the air, g;
m 2 is the mass, g, of the oil-containing (fully immersed) sample weighed in air;
ρ is the density, g/cm, of the oil for immersion 3 ；
V is the sample volume, cm 3 。
2. Average pore diameter: the average pore size is measured according to the test standard of the measurement of the average pore size of flow in a permeable sintered metal material of GBT 38516-2020, in combination with the test of the pore size of a bubble test and the gas permeability:
wherein:
gamma is the test liquid surface tension, see GB/T5249, N/m;
Δp is the medium flow differential pressure, pa.
3. Hardness: the average value was measured at 5 points using a micro Vickers hardness tester (HXS-1000 AY) with a loading of 9.8N and a loading time of 15 s.
4. Surface roughness: a hand-held surface roughness measuring instrument (TR 200) is used, 5 points are randomly taken from the surface to be measured, and an average value is taken.
Table 1: and (5) testing the performance of the porous copper-zinc binary alloy.
As can be seen from fig. 3 and 4, the hole patterns were changed from irregular sheets to spherical shapes after pore sphericizing treatment of the sintered compact in example 1, as compared with comparative example 1; as can be seen from fig. 5 to 8 and table 1, in example 1, after spheroidizing the pores, the hardness of the porous alloy is significantly improved as compared with that in comparative example 1, and the workability is also significantly improved, the roughness of the machined surface is significantly reduced, and the chip is broken in a chipping shape. Meanwhile, the porosity of the porous spheroidized material in example 1 is not affected compared with that of the porous spheroidized material in comparative example 1, and the ability of the material to leak stamp pad ink is not affected, so that the material is suitable for processing seals.
However, the temperature at the time of spheroidizing the pores in comparative example 2 was too low to achieve the spheroidizing effect, failing to spheroidize the irregular pores, resulting in a significant decrease in hardness and workability of the material as compared with example 1; the pore spheroidization in comparative example 3 was too high in temperature, and although the pores were spheroidized, the cutting performance was improved, but the porosity and pore diameter were remarkably reduced, and the leakage of stamp pad ink was not facilitated when it was used for making a stamp, and at the same time, the too high temperature led to volatilization of zinc.
Claims (10)
1. The preparation method of the free-cutting porous copper-zinc binary alloy for the seal is characterized by comprising the following steps of:
(1) Drying the copper-zinc alloy powder and pressing the dried copper-zinc alloy powder into a pressed compact;
(2) Carrying out reduction treatment on the obtained pressed compact in a reducing atmosphere;
(3) Sintering the reduced pressed compact in a protective atmosphere at 650-800 ℃ to obtain a sintered body with a pore structure;
(4) And (3) performing pore spheroidization on the sintered body in a protective atmosphere, wherein the temperature of pore spheroidization is 450-600 ℃, and obtaining the free-cutting porous copper-zinc binary alloy for the seal.
2. The preparation method according to claim 1, wherein the mass ratio of copper to zinc in the copper-zinc alloy powder in the step (1) is 1.25 to 1.63, and the particle size of the copper-zinc alloy powder is 40 to 150 μm.
3. The preparation method according to claim 2, wherein the mass ratio of copper to zinc in the copper-zinc alloy powder is 1.42-1.57.
4. The preparation method according to claim 1 or 2, wherein the drying in step (1) is carried out by low-temperature vacuum drying at 50-80 ℃ and 10 vacuum degree -3 ～10 -5 Pa, and drying time is 5-15 h.
5. The preparation method according to claim 1 or 2, wherein the pressing in the step (1) adopts a limit pressing mode, the height compression ratio is 1.5-2.5, and the dwell time is 3-10 s.
6. The process according to claim 5, wherein the high compression ratio is 1.7 to 2.3.
7. The method according to claim 1, wherein the reducing atmosphere in the step (2) is hydrogen, and the dew point of the reducing atmosphere is lower than 0 ℃; the temperature during the reduction treatment is 250-450 ℃, the temperature rising rate is 1-5 ℃/min, and the heat preservation time is 0.5-5 h.
8. The method according to claim 1, wherein the protective atmosphere in the step (3) is one selected from the group consisting of hydrogen, nitrogen and argon; the temperature rising rate during sintering is 1-10 ℃/min, the heat preservation time is 1-3 h, and the temperature is reduced along with the furnace.
9. The process according to claim 1 or 8, wherein the sintered body obtained in the step (3) has a porosity of 5 to 30% and a pore size of 5 to 50. Mu.m.
10. The method according to claim 1, wherein the protective atmosphere in the step (4) is one selected from the group consisting of hydrogen, nitrogen and argon; the heat preservation time of pore spheroidization is 0.5-3 h, and the pore spheroidization is cooled along with a furnace.
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| US5019311A (en) * | 1989-02-23 | 1991-05-28 | Koslow Technologies Corporation | Process for the production of materials characterized by a continuous web matrix or force point bonding |
| KR20020060018A (en) * | 2001-01-09 | 2002-07-16 | 손인국 | Brass alloy for cutting tool with high speed performance |
| JP2005154866A (en) * | 2003-11-27 | 2005-06-16 | Nippon Kagaku Yakin Co Ltd | Cu BASED ALLOY FOR THERMAL CONDUCTION, AND ITS PRODUCTION METHOD |
| CN106676307A (en) * | 2016-04-15 | 2017-05-17 | 中南大学 | Preparing method of copper sintered porous material |
| CN108149048A (en) * | 2017-12-25 | 2018-06-12 | 西安理工大学 | Micro-nano twin-stage Porous Cu and preparation method thereof |
| CN109112352A (en) * | 2018-09-11 | 2019-01-01 | 广东美的制冷设备有限公司 | Foamed alloy and its preparation method and application for air conditioner sound-deadening and noise-reducing |
| US20210040989A1 (en) * | 2018-01-29 | 2021-02-11 | Porite Corporation | Sintered bearing and method for manufacturing sintered bearing |
| CN115416410A (en) * | 2022-08-30 | 2022-12-02 | 浙江省冶金研究院有限公司 | Porous metal seal |
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2022
- 2022-12-20 CN CN202211641523.5A patent/CN116262952B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5019311A (en) * | 1989-02-23 | 1991-05-28 | Koslow Technologies Corporation | Process for the production of materials characterized by a continuous web matrix or force point bonding |
| KR20020060018A (en) * | 2001-01-09 | 2002-07-16 | 손인국 | Brass alloy for cutting tool with high speed performance |
| JP2005154866A (en) * | 2003-11-27 | 2005-06-16 | Nippon Kagaku Yakin Co Ltd | Cu BASED ALLOY FOR THERMAL CONDUCTION, AND ITS PRODUCTION METHOD |
| CN106676307A (en) * | 2016-04-15 | 2017-05-17 | 中南大学 | Preparing method of copper sintered porous material |
| CN108149048A (en) * | 2017-12-25 | 2018-06-12 | 西安理工大学 | Micro-nano twin-stage Porous Cu and preparation method thereof |
| US20210040989A1 (en) * | 2018-01-29 | 2021-02-11 | Porite Corporation | Sintered bearing and method for manufacturing sintered bearing |
| CN109112352A (en) * | 2018-09-11 | 2019-01-01 | 广东美的制冷设备有限公司 | Foamed alloy and its preparation method and application for air conditioner sound-deadening and noise-reducing |
| CN115416410A (en) * | 2022-08-30 | 2022-12-02 | 浙江省冶金研究院有限公司 | Porous metal seal |
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