CN103820671A - High-hardness pure gold material and preparation method thereof - Google Patents
High-hardness pure gold material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-purity and high-hardness gold alloy material which comprises the following components: cobalt, stibium, scandium, gold and impurities. A preparation method of the high-purity and high-hardness gold alloy material comprises the following steps that a, a gold-cobalt intermediate alloy is prepared; b, a gold-stibium intermediate alloy is prepared; c, a gold-scandium intermediate alloy is prepared; d, blending is performed; e, the blended intermediate alloys are mixed uniformly and placed at the bottom of a first copper crucible in a vacuum arc furnace; Au9999 pure gold is laid above; a titanium ball is placed in a second copper crucible; a furnace door is closed; first vacuumizing is performed; argon is filled; second vacuumizing is performed; argon is filled; f, residual oxygen is removed; a material in the first copper crucible is molten down; current is adjusted; a magnetic stirring power supply is started and kept for 1-1.5min; the power supply is cut off; molten metal is solidified; and h, a cast ingot is subjected to solution treatment, refreezing processing and aging treatment. A pure gold alloy prepared via the method is fine in crystal grain and high in hardness, and a precipitated phase is diffused and distributed in a substrate.
Description
Technical field
The present invention relates to a kind of high rigidity pure gold material and preparation method thereof.
Background technology
Chinese wear the existing thousands of years history of gold jewelry, are all to advocate high-purity gold ornaments (according to ISO9202:1991, pure gold refers to that gold content is not less than the au-alloy of 99.0wt%, and thousand pure golds refer to that gold content is not less than the au-alloy of 99.9wt%) for a long time.After gold ornaments market access, traditional oriental cultural and consumption preference do not change, and solid gold jewelry still keeps lion's share in gold consumption.But there are some distinct issues in traditional solid gold jewelry in manufacture and use procedure.Due to pure gold hardness very low (only having HV27 under annealed state), be difficult to meet high-precision processing technology of jewelry, be difficult to embedding gem, the fashion style of complex process is difficult to carry out, difficulty makes that moulding complexity, decorative pattern are careful, the jewellery of through-carved work, cause highly purified gold ornament all the time in the awkward condition extensive, artistry is not enough, expand and exist certain limitation in the exploitation of gold jewelry, greatly restricted the artistic value of proof gold product as luxury goods.Use aspect ornaments wearing, due to hardness undercapacity, ornaments are easily out of shape, easily wearing and tearing and tarnishing of surface.Along with the raising of domestic material and cultural life, human consumer is also higher to the requirement of pure gold ornaments, not only will guarantee high quality, also there is to higher expectation the aspect such as structure style and use properties of ornaments.Therefore, pure gold material is carried out to modification, exploitation the Gold Content high strength, high rigidity solid gold jewelry material and the production technique that meet the demands, become new focus and the urgent need to solve the problem of decorations high-purity gold research field.
Some researchists, exploring and attempt aspect research high strength pure gold material, mainly contain the alloy systems such as Au-Ti, Au-Zr, Au-RE both at home and abroad.The people such as Geoffrey Gafner have proposed to strengthen pure gold with titanium the earliest, and develop 990Au-10Ti alloy, it is a kind of alloy with age hardening ability, be golden yellow, there is certain antiwear property, become the important foundation of pure gold study on the modification in recent years, much research is afterwards all further to improve on the basis of Au-Ti system.But because this alloy contains more titanium, melting technology complexity, and also the color of alloy has certain influence.Au-Zr system is also one of more modification pure gold of foreign study, in pure gold, add zirconium and have two kinds of strengthening mechanisms: the one, form the dispersion-strengthened of zirconium disperse educt phase by ag(e)ing process, the 2nd, form the solution strengthening of substitutional solid solution, compared with titanium, the impact of the interpolation alloy color of zirconium is little, but its concentration slightly Gao Shiyi cause alloy embrittlement.It is, with rare earth element, gold is carried out to modification that Au-RE is associated gold, result of study shows that rare earth element adds the effect that can play crystal grain thinning in gold, when as cast condition, can form refractory oxide becomes the forming core core of alloy, in annealing process, can separate out prevention grain growth at crystal boundary, be effective grain-refining agent, can improve the strength property of pure gold.In general, after pure gold modification, obtain certain effect, intensity hardness has raising in various degree, but also there are many problems, main manifestations is: strength property deficiency, and some modification pure gold is processed by all means rear final hardness and is also only had HV60 left and right, and some pure gold work hardness can reach HV110, but easily there is natural ageing and softening situation, be difficult to meet and produce and service requirements; The color and luster of some modification pure gold is not good, in use easily occurs intense darkness without light problem; The working condition harshness of some modification pure gold.
Summary of the invention
The object of the present invention is to provide a kind of high rigidity pure gold material and preparation method thereof.
The technical solution used in the present invention is:
A kind of high rigidity pure gold material, it is to be made up of the component of following content:
0.15-0.30%wt cobalt, 0.12-0.29%wt antimony, 0.10-0.18%wt scandium, golden 99.22-99.65% and other inevitable impurity surplus.
A preparation method for high rigidity pure gold material, comprises the following steps:
A. prepare golden cobalt master alloy: press (94-96): the melting in vacuum arc fumace by Au9999 proof gold and the pure cobalt of Co9998 of 1 mass ratio, makes golden cobalt master alloy;
B. prepare golden antimony master alloy: (89-91) in mass ratio: 1 melting in vacuum arc fumace by Au9999 proof gold and Sb9999 star antimony, makes golden antimony master alloy;
C. prepare golden bearing master alloy: press (89-91): the melting in vacuum arc fumace by Au9999 proof gold and the pure scandium of Sc9999 of 1 mass ratio, makes golden bearing master alloy;
D. batching: golden bearing master alloy, the Au9999 proof gold prepared in the golden antimony master alloy of preparing in the golden cobalt master alloy of preparing in step a, step b, step c are cut into particle and prepare burden as raw material, ingredients principle is: after batching, to make in the product of the last gained of this preparation method, the mass percent of cobalt element is 0.15-0.30%, the mass percent of antimony element is 0.12-0.29%, the mass percent of scandium element is 0.10-0.18%, gold element 99.22-99.65% and other inevitable impurity surplus;
E, the golden cobalt master alloy that upper step is prepared burden, golden antimony master alloy, golden bearing master alloy mix and are placed on the bottom of the first copper crucible in vacuum arc fumace, then on lay, walk the Au9999 proof gold of having prepared burden in the above; In the second copper crucible, place titanium ball, closed furnace door, vacuumizes for the first time, is then filled with for the first time argon gas; Vacuumize for the second time, be then filled with for the second time argon gas;
F, with first melt titanium ball after 60 ~ 70A current arc ignition to remove residual oxygen, then arc flame is aimed to the material in the first copper crucible, adjustment electric current is 90 ~ 100A, after the material in the first copper crucible melts clearly, adjustment electric current is 80 ~ 90A, start magnetic and stir power supply, keep 1 ~ 1.5min, then power-off molten metal is solidified;
G, by repeatedly carrying out again operation 2-3 time of step f after the ingot overturning after solidifying, finally electric current is adjusted to 90 ~ 100A, moltenly remove arc flame after clear, make molten metal be frozen into ingot casting in water-cooled copper ingot mould;
H, ingot casting that upper step is obtained be 650 ~ 750 ℃ of solution treatment, then carry out cold working, then at 200 ~ 300 ℃ of ageing treatment 3 ~ 12h.
In steps d, the particle diameter of described particle is at 1-5mm.
In step e, the particle diameter of described titanium ball is 10-15mm.
In step e, be evacuated to for the first time 3 × 10
-3pa, is filled with argon gas to 0.8 ~ 1atm for the first time.
In step e, be evacuated to for the second time 3 × 10
-3pa, is filled with argon gas to 1 ~ 1.1atm for the second time.
In step h, described cold working is roll compacting, drawing, punching press.
The invention has the beneficial effects as follows: the present invention by vacuum arc melting, Quench solidify, the aggregate measures such as solution treatment, working hardening, ageing treatment, the pure gold alloy grain making is tiny, precipitated phase disperse is distributed in matrix.Pure gold hardness after modification significantly improves, and brightness is higher than Au9999, and colourity is substantially approaching, and solidity to corrosion remains unchanged substantially.
Accompanying drawing explanation
Fig. 1 is the work hardening behavior contrast of high rigidity pure gold of the present invention and Au9999;
Fig. 2 is the ag(e)ing behavio(u)r of high rigidity pure gold of the present invention;
Fig. 3 is the micro-organization chart of high rigidity gold pure gold of the present invention;
Fig. 4 is the micro-organization chart of Au9999;
Fig. 5 is the distribution plan of cobalt in substrate in high rigidity pure gold of the present invention;
Fig. 6 is the distribution plan of antimony in substrate in high rigidity pure gold of the present invention;
Fig. 7 is the distribution plan of scandium in substrate in high rigidity pure gold of the present invention;
Fig. 8 is polarization curve and the Au9999 comparison diagram of high rigidity pure gold of the present invention in synthetic perspiration.
Embodiment
A kind of high rigidity pure gold material, it is to be made up of the component of following content:
0.15-0.30%wt cobalt, 0.12-0.29%wt antimony, 0.10-0.18%wt scandium, golden 99.22-99.65%wt and other inevitable impurity surplus.
A preparation method for high rigidity pure gold material, comprises the following steps:
A. prepare golden cobalt master alloy: press (94-96): the melting in vacuum arc fumace by Au9999 proof gold and the pure cobalt of Co9998 of 1 mass ratio, makes golden cobalt master alloy;
B. prepare golden antimony master alloy: (89-91) in mass ratio: 1 melting in vacuum arc fumace by Au9999 proof gold and Sb9999 star antimony, makes golden antimony master alloy;
C. prepare golden bearing master alloy: press (89-91): the melting in vacuum arc fumace by Au9999 proof gold and the pure scandium of Sc9999 of 1 mass ratio, makes golden bearing master alloy;
D. batching: golden bearing master alloy, the Au9999 proof gold prepared in the golden antimony master alloy of preparing in the golden cobalt master alloy of preparing in step a, step b, step c are cut into particle and prepare burden as raw material, ingredients principle is: after batching, to make in the product of the last gained of this preparation method, the mass percent of cobalt element is 0.15-0.30%, the mass percent of antimony element is 0.12-0.29%, the mass percent of scandium element is 0.10-0.18%, and the mass percent of gold element is 99.22-99.65% and other inevitable impurity surplus;
E, the golden cobalt master alloy that upper step is prepared burden, golden antimony master alloy, golden bearing master alloy mix and are placed on the bottom of the first copper crucible in vacuum arc fumace, then on lay, walk the Au9999 proof gold of having prepared burden in the above; In the second copper crucible, place titanium ball, closed furnace door, vacuumizes for the first time, is then filled with for the first time argon gas; Vacuumize for the second time, be then filled with for the second time argon gas;
F, with first melt titanium ball after 60 ~ 70A current arc ignition to remove residual oxygen, then arc flame is aimed to the material in the first copper crucible, adjustment electric current is 90 ~ 100A, after the material in the first copper crucible melts clearly, adjustment electric current is 80 ~ 90A, start magnetic and stir power supply, keep 1 ~ 1.5min, then power-off molten metal is solidified;
G, by repeatedly carrying out again operation 2-3 time of step f after the ingot overturning after solidifying, finally electric current is adjusted to 90 ~ 100A, moltenly remove arc flame after clear, make molten metal be frozen into ingot casting in water-cooled copper ingot mould;
H, ingot casting that upper step is obtained be 650 ~ 750 ℃ of solution treatment, then carry out cold working, then at 200 ~ 300 ℃ of ageing treatment 3 ~ 12h.
In steps d, the particle diameter of described particle is at 1-5mm.
In step e, the particle diameter of described titanium ball is 10-15mm.
In step e, be evacuated to for the first time 3 × 10
-3pa, is filled with argon gas to 0.8 ~ 1atm for the first time.
In step e, be evacuated to for the second time 3 × 10
-3pa, is filled with argon gas to 1 ~ 1.1atm for the second time.
In step h, described cold working is roll compacting, drawing, punching press.
Below in conjunction with specific embodiment, the present invention is described further:
embodiment 1:
The preparation method of the high rigidity pure gold of the present embodiment, comprises the following steps:
A. be Au9999 proof gold by mass ratio: the proof gold of the pure cobalt=95:1 of Co9998 and the melting in vacuum arc fumace of pure cobalt, make golden cobalt master alloy.
B. be Au9999 proof gold by mass ratio: the melting in vacuum arc fumace of the proof gold of Sb9999 star antimony=90:1 and star antimony, makes golden antimony master alloy.
C. be Au9999 proof gold by mass ratio: the proof gold of the pure scandium=90:1 of Sc9999 and the melting in vacuum arc fumace of pure scandium, make golden bearing master alloy.
D. the golden cobalt master alloy that is 25% according to mass percent, 21% golden antimony master alloy, 17% golden bearing master alloy, all the other are Au9999 proof gold batching, and described starting material all pass through to shred and are all fine granularity (particle diameter is 1-5mm).
E. golden cobalt master alloy, golden antimony master alloy, golden bearing master alloy are placed on to the bottom of the copper crucible of vacuum arc casting room, then place Au9999 proof gold in the above.Place titanium ball (titanium spherical diameter is 15mm) at another copper crucible center, closed furnace door, is evacuated down to 1.4 × 10
-3pa, is then filled with argon gas to 0.9atm, is again evacuated down to 1.4 × 10
-3pa, and then be filled with argon gas to 1.05atm.To remove the residual oxygen of possibility, then arc flame is aimed to raw material in copper crucible with first melt titanium ball after 65A current arc ignition, adjustment electric current is 95A, after raw material melts clearly, adjustment electric current is 85A, starts magnetic and stirs power supply, keep 1.3min, then have a power failure molten metal is solidified.By melting again after ingot overturning, 3 times repeatedly, finally electric current is adjusted to 95A, remove rapidly arc flame after molten clear, make molten metal be frozen into ingot in water-cooled copper ingot mould.
F. the pure gold ingot casting of preparation, 700 ℃ of solution treatment, then carries out cold working by the mode of roll compacting, drawing, punching press, then at 250 ℃ of ageing treatment 6h.
High rigidity pure gold prepared by the present embodiment, through measuring, its composition is made up of following component by weight percentage:
Cobalt 0.25%, antimony 0.20%, scandium 0.15%, gold 99.39% and inevitable impurity surplus.
The high rigidity pure gold that the present embodiment makes, Gold Content is 99.39%, and hardness of cast form reaches HV62, and after 700 ℃ of solution treatment, solid solution state hardness reaches HV51, and Au9999 only has HV 27.Solid solution state material is carried out to roll compacting distortion, and single process amount approximately 20%, detects hardness after each processing, and contrasts with Au9999 material, sees accompanying drawing 1.When the cold deformation quantity of modification pure gold material of solid solution state is 80%, hardness can reach HV121, and Au9999 only has HV73.Material after cold working is carried out to ageing treatment, and its hardness is shown in accompanying drawing 2 with the Changing Pattern of aging temp and aging time, the highest the timeliness hardness of 250 ℃, can reach HV138.Under scanning electron microscope, observe the microstructure of the alloy of the present embodiment, and contrast with Au9999 material, see accompanying drawing 3-4, both present obvious single solid solution structure, wherein visible part twin structure, this metallographic has presented the good face-centred cubic structure feature of recrystallize, but the crystal grain of the present embodiment alloy is thinner than Au9999, illustrate that micro-cobalt, antimony, scandium and quickening solidification cooling can play effective Grain Refinement Effect, this refining effect contributes to put forward heavy alloyed intensity and hardness.Through micro-area composition scanning analysis, cobalt, antimony, the main disperse of scandium are distributed in matrix, do not form obvious segregation phenomenon, see accompanying drawing 5-7.With the polarization behavior of LK2005A electrochemical workstation test material, see accompanying drawing 8, the pitting potential of Au9999 in 37 ℃ of synthetic perspirations is 1.19V, and the pitting potential of the present embodiment alloy is 1.17V, pitting resistance aspect does not almost affect.The color coordinates value of modification pure gold material and Au9999 sees attached list 1, and both colourimetric number a* and b* are very approaching, but the brightness value of modified alloy is obviously better than Au9999, and this is highly beneficial for obtaining highlighted surface effect.
Table 1
embodiment 2:
The preparation method of the high rigidity pure gold of the present embodiment, comprises the following steps:
A. be Au9999 proof gold by mass ratio: the proof gold of the pure cobalt=95:1 of Co9998 and the melting in vacuum arc fumace of pure cobalt, make golden cobalt master alloy.
B. be to be Au9999 proof gold by mass ratio by mass ratio: the melting in vacuum arc fumace of the proof gold of Sb9999 star antimony=90:1 and star antimony, makes golden antimony master alloy.
C. be Au9999 proof gold by mass ratio: the proof gold of the pure scandium=90:1 of Sc9999 and the melting in vacuum arc fumace of pure scandium, make golden bearing master alloy.
D. the golden cobalt master alloy that is 11% according to mass percent, 12% golden antimony master alloy, 11% golden bearing master alloy, all the other are Au9999 proof gold batching, and described starting material are all fine granularity.
E. golden cobalt master alloy, golden antimony master alloy, golden bearing master alloy are placed on to the bottom of the copper crucible of vacuum arc casting room, then place Au9999 proof gold in the above.Place titanium ball at copper crucible center, closed furnace door, is evacuated down to 1.8 × 10
-3pa, is then filled with argon gas to 0.86atm, is again evacuated down to 1.8 × 10
-3pa, and then be filled with argon gas to 1.03atm.To remove the residual oxygen of possibility, then arc flame is aimed to raw material in copper crucible with first melt titanium ball after 66A current arc ignition, adjustment electric current is 90A, after raw material melts clearly, adjustment electric current is 87A, starts magnetic and stirs power supply, keep 1.4min, then have a power failure molten metal is solidified.By melting again after ingot overturning, 3 times repeatedly, finally electric current is adjusted to 98A, remove rapidly arc flame after molten clear, make molten metal be frozen into ingot in water-cooled copper ingot mould.
F. the pure gold ingot casting of preparation, 700 ℃ of solution treatment, then carries out cold working by the mode of roll compacting, drawing, punching press, then at 250 ℃ of ageing treatment 6h.
High rigidity pure gold prepared by the present embodiment, through measuring, its composition is made up of following component by weight percentage:
Cobalt 0.11%, antimony 0.12%, scandium 0.10%, gold 99.65%, inevitable impurity surplus.
The high-purity high rigidity au-alloy that the present embodiment makes, Gold Content is 99.65%, and hardness of cast form reaches HV58, and after 700 ℃ of solution treatment, solid solution state hardness reaches HV46, and Au9999 only has HV 27.Solid solution state material is carried out to roll compacting distortion, single process amount approximately 20%, when cold deformation quantity is 80%, modification pure gold material hardness can reach HV111.Material after cold working is carried out to ageing treatment, can reach HV126 the timeliness hardness of 250 ℃.Under scanning electron microscope, observe the microstructure of the alloy of the present embodiment, present obvious single solid solution structure, crystal grain is tiny, and wherein visible part twin structure has presented the good face-centred cubic structure feature of recrystallize, contributes to put forward heavy alloyed intensity and hardness.Through micro-area composition scanning analysis, cobalt, antimony, the main disperse of scandium are distributed in matrix, do not form obvious segregation phenomenon.With the polarization behavior of LK2005A electrochemical workstation test material, the pitting potential of the present embodiment alloy is 1.18V, approaches very much Au9999, and pitting resistance aspect does not almost affect.The colourimetric number a* of the present embodiment alloy and b* and Au9999 are very approaching, and brightness value approximately exceeds 4 than Au9999, is conducive to obtain highlighted surface effect.
embodiment 3:
The preparation method of the high rigidity pure gold of the present embodiment, comprises the following steps:
A. be Au9999 proof gold by mass ratio: the proof gold of the pure cobalt=95:1 of Co9998 and the melting in vacuum arc fumace of pure cobalt, the golden cobalt master alloy that to make containing weight of cobalt per-cent be 1.01%.
B. by mass ratio for being Au9999 proof gold by mass ratio: the melting in vacuum arc fumace of the proof gold of Sb9999 star antimony=90:1 and star antimony, the golden antimony master alloy that to make containing antimony weight percent be 1.03%.
C. be Au9999 proof gold by mass ratio: the proof gold of the pure scandium=90:1 of Sc9999 and the melting in vacuum arc fumace of pure scandium, the golden bearing master alloy that to make containing scandium weight ratio be 0.98%.
D. the golden cobalt master alloy that is 31% according to mass percent, 30% golden antimony master alloy, 20% golden bearing master alloy, all the other are Au9999 proof gold batching, and described starting material are all fine granularity.
E. golden cobalt master alloy, golden antimony master alloy, golden bearing master alloy are placed on to the bottom of the copper crucible of vacuum arc casting room, then place Au9999 proof gold in the above.Place titanium ball at copper crucible center, closed furnace door, is evacuated down to 1.2 × 10
-3pa, is then filled with argon gas to 0.9atm, is again evacuated down to 1.2 × 10
-3pa, and then be filled with argon gas to 1.05atm.To remove the residual oxygen of possibility, then arc flame is aimed to raw material in copper crucible with first melt titanium ball after 70A current arc ignition, adjustment electric current is 95A, after raw material melts clearly, adjustment electric current is 90A, starts magnetic and stirs power supply, keep 1.5min, then have a power failure molten metal is solidified.By melting again after ingot overturning, 3 times repeatedly, finally electric current is adjusted to 95A, remove rapidly arc flame after molten clear, make molten metal be frozen into ingot in water-cooled copper ingot mould.
F. the pure gold ingot casting of preparation, 700 ℃ of solution treatment, then carries out cold working by the mode of roll compacting, drawing, punching press, then at 250 ℃ of ageing treatment 6h.
High rigidity pure gold prepared by the present embodiment, through measuring, its composition is made up of following component by weight percentage:
Cobalt 0.30%, antimony 0.29%, scandium 0.18%, gold 99.22%, inevitably impurity surplus.
The high-purity high rigidity au-alloy that the present embodiment makes, Gold Content is 99.22%, and hardness of cast form reaches HV65, and after 700 ℃ of solution treatment, solid solution state hardness reaches HV57, and Au9999 only has HV 27.Solid solution state material is carried out to roll compacting distortion, single process amount approximately 20%, when cold deformation quantity is 80%, modification pure gold material hardness can reach HV129.Material after cold working is carried out to ageing treatment, can reach HV146 the timeliness hardness of 250 ℃.Under scanning electron microscope, observe the microstructure of the alloy of the present embodiment, present obvious single solid solution structure, crystal grain is tiny, and wherein visible part twin structure has presented the good face-centred cubic structure feature of recrystallize, contributes to put forward heavy alloyed intensity and hardness.Through micro-area composition scanning analysis, cobalt, antimony, the main disperse of scandium are distributed in matrix, do not form obvious segregation phenomenon.With the polarization behavior of LK2005A electrochemical workstation test material, the pitting potential of the present embodiment alloy is 1.16V, approaches very much Au9999, and pitting resistance aspect does not almost affect.The colourimetric number a* of the present embodiment alloy and b* and Au9999 are very approaching, and brightness value approximately exceeds 5 than Au9999, is conducive to obtain highlighted surface effect.
embodiment 4:
The preparation method of the high rigidity pure gold of the present embodiment, comprises the following steps:
A. be Au9999 proof gold by mass ratio: the proof gold of the pure cobalt=95:1 of Co9998 and the melting in vacuum arc fumace of pure cobalt, the golden cobalt master alloy that to make containing weight of cobalt per-cent be 1.01%.
B. by mass ratio for being Au9999 proof gold by mass ratio: the melting in vacuum arc fumace of the proof gold of Sb9999 star antimony=90:1 and star antimony, the golden antimony master alloy that to make containing antimony weight percent be 1.03%.
C. be Au9999 proof gold by mass ratio: the proof gold of the pure scandium=90:1 of Sc9999 and the melting in vacuum arc fumace of pure scandium, the golden bearing master alloy that to make containing scandium weight ratio be 0.98%.
D. the golden cobalt master alloy that is 15% according to mass percent, 22% golden antimony master alloy, 14% golden bearing master alloy, all the other are Au9999 proof gold batching, and described starting material are all fine granularity.
E. golden cobalt master alloy, golden antimony master alloy, golden bearing master alloy are placed on to the bottom of the copper crucible of vacuum arc casting room, then place Au9999 proof gold in the above.Place titanium ball at copper crucible center, closed furnace door, is evacuated down to 1.5 × 10
-3pa, is then filled with argon gas to 0.88atm, is again evacuated down to 1.5 × 10
-3pa, and then be filled with argon gas to 1.03atm.To remove the residual oxygen of possibility, then arc flame is aimed to raw material in copper crucible with first melt titanium ball after 66A current arc ignition, adjustment electric current is 92A, after raw material melts clearly, adjustment electric current is 87A, starts magnetic and stirs power supply, keep 1.4min, then have a power failure molten metal is solidified.By melting again after ingot overturning, 3 times repeatedly, finally electric current is adjusted to 90A, remove rapidly arc flame after molten clear, make molten metal be frozen into ingot in water-cooled copper ingot mould.
F. the pure gold ingot casting of preparation, 700 ℃ of solution treatment, then carries out cold working by the mode of roll compacting, drawing, punching press, then at 250 ℃ of ageing treatment 6h.
High rigidity pure gold prepared by the present embodiment, through measuring, its composition is made up of following component by weight percentage:
Cobalt 0.15%, antimony 0.21%, scandium 0.12%, gold 99.50%, surplus is inevitable impurity.
The high-purity high rigidity au-alloy that the present embodiment makes, Gold Content is 99.50%, and hardness of cast form reaches HV61, and after 700 ℃ of solution treatment, solid solution state hardness reaches HV50, and Au9999 only has HV 27.Solid solution state material is carried out to roll compacting distortion, single process amount approximately 20%, when cold deformation quantity is 80%, modification pure gold material hardness can reach HV119.Material after cold working is carried out to ageing treatment, can reach HV134 the timeliness hardness of 250 ℃.Under scanning electron microscope, observe the microstructure of the alloy of the present embodiment, present obvious single solid solution structure, crystal grain is tiny, and wherein visible part twin structure has presented the good face-centred cubic structure feature of recrystallize, contributes to put forward heavy alloyed intensity and hardness.Through micro-area composition scanning analysis, cobalt, antimony, the main disperse of scandium are distributed in matrix, do not form obvious segregation phenomenon.With the polarization behavior of LK2005A electrochemical workstation test material, the pitting potential of the present embodiment alloy is 1.18V, approaches very much Au9999, and pitting resistance aspect does not almost affect.The colourimetric number a* of the present embodiment alloy and b* and Au9999 are very approaching, and brightness value approximately exceeds 5 than Au9999, is conducive to obtain highlighted surface effect.
Although finally explanation be, above embodiment only in order to technical scheme of the present invention to be described unrestricted with reference to preferred embodiment to the present invention have been described in detail, those of ordinary skill in the art is to be understood that, can to technical scheme of the present invention modify or be equal to replace and do not depart from the aim of technical solution of the present invention and scope, it all should be encompassed in the middle of claim scope of the present invention.
Claims (7)
1. a high rigidity pure gold material, is characterized in that: it is to be made up of the component of following content:
0.15-0.30%wt cobalt, 0.12-0.29%wt antimony, 0.10-0.18%wt scandium, golden 99.22-99.65% and other inevitable impurity surplus.
2. the preparation method of a kind of high rigidity pure gold material claimed in claim 1, is characterized in that: comprise the following steps:
A. prepare golden cobalt master alloy: press (94-96): the melting in vacuum arc fumace by Au9999 proof gold and the pure cobalt of Co9998 of 1 mass ratio, makes golden cobalt master alloy;
B. prepare golden antimony master alloy: (89-91) in mass ratio: 1 melting in vacuum arc fumace by Au9999 proof gold and Sb9999 star antimony, makes golden antimony master alloy;
C. prepare golden bearing master alloy: press (89-91): the melting in vacuum arc fumace by Au9999 proof gold and the pure scandium of Sc9999 of 1 mass ratio, makes golden bearing master alloy;
D. batching: golden bearing master alloy, the Au9999 proof gold prepared in the golden antimony master alloy of preparing in the golden cobalt master alloy of preparing in step a, step b, step c are cut into particle and prepare burden as raw material, ingredients principle is: after batching, to make in the product of the last gained of this preparation method, the mass percent of cobalt element is 0.15-0.30%, the mass percent of antimony element is 0.12-0.29%, the mass percent of scandium element is 0.10-0.18%, gold element 99.22-99.65% and other inevitable impurity surplus;
E, the golden cobalt master alloy that upper step is prepared burden, golden antimony master alloy, golden bearing master alloy mix and are placed on the bottom of the first copper crucible in vacuum arc fumace, then on lay, walk the Au9999 proof gold of having prepared burden in the above; In the second copper crucible, place titanium ball, closed furnace door, vacuumizes for the first time, is then filled with for the first time argon gas; Vacuumize for the second time, be then filled with for the second time argon gas;
F, with first melt titanium ball after 60 ~ 70A current arc ignition to remove residual oxygen, then arc flame is aimed to the material in the first copper crucible, adjustment electric current is 90 ~ 100A, after the material in the first copper crucible melts clearly, adjustment electric current is 80 ~ 90A, start magnetic and stir power supply, keep 1 ~ 1.5min, then power-off molten metal is solidified;
G, by repeatedly carrying out again operation 2-3 time of step f after the ingot overturning after solidifying, finally electric current is adjusted to 90 ~ 100A, moltenly remove arc flame after clear, make molten metal be frozen into ingot casting in water-cooled copper ingot mould;
H, ingot casting that upper step is obtained be 650 ~ 750 ℃ of solution treatment, then carry out cold working, then at 200 ~ 300 ℃ of ageing treatment 3 ~ 12h.
3. the preparation method of a kind of high rigidity pure gold material according to claim 2, is characterized in that: in steps d, the particle diameter of described particle is at 1-5mm.
4. the preparation method of a kind of high rigidity pure gold material according to claim 2, is characterized in that: in step e, the particle diameter of described titanium ball is 10-15mm.
5. the preparation method of a kind of high rigidity pure gold material according to claim 2, is characterized in that: in step e, be evacuated to for the first time 3 × 10
-3pa, is filled with argon gas to 0.8 ~ 1atm for the first time.
6. the preparation method of a kind of high rigidity pure gold material according to claim 2, is characterized in that: in step e, be evacuated to for the second time 3 × 10
-3pa, is filled with argon gas to 1 ~ 1.1atm for the second time.
7. the preparation method of a kind of high rigidity pure gold material according to claim 2, is characterized in that: in step h, described cold working is roll compacting, drawing, punching press.
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| CN106636721A (en) * | 2015-10-30 | 2017-05-10 | 深圳市周大福珠宝制造有限公司 | Gold alloy |
| CN109373755A (en) * | 2018-10-14 | 2019-02-22 | 昆山建金工业设计有限公司 | A kind of device of gold element and antimony element composite material |
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Cited By (2)
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| CN106636721A (en) * | 2015-10-30 | 2017-05-10 | 深圳市周大福珠宝制造有限公司 | Gold alloy |
| CN109373755A (en) * | 2018-10-14 | 2019-02-22 | 昆山建金工业设计有限公司 | A kind of device of gold element and antimony element composite material |
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