CN106702244B - A kind of hard pure gold opening-supplementing material and preparation method thereof - Google Patents
A kind of hard pure gold opening-supplementing material and preparation method thereof Download PDFInfo
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- CN106702244B CN106702244B CN201611128923.0A CN201611128923A CN106702244B CN 106702244 B CN106702244 B CN 106702244B CN 201611128923 A CN201611128923 A CN 201611128923A CN 106702244 B CN106702244 B CN 106702244B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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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
- C22C1/02—Making non-ferrous alloys by melting
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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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/02—Alloys based on gold
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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Abstract
The present invention provides a kind of hard pure gold opening-supplementing material and preparation method thereof, which includes following component and percentage by weight：Dysprosium 60% ~ 85%, indium 10% ~ 15%, zinc 0.5% ~ 10%, cobalt 2% ~ 10%；The weight proportion of dysprosium and two kinds of elements of indium is 84 ~ 86:14~16.The present invention is used as main intensified element using dysprosium doping, its the second phase hardening thing is Au4Dy, collocation phosphide element makes the fusion temperature of dysprosium be down to 1100 DEG C, ensure that it adapts to conventional noble metal jewelry smelting technology, add zinc and improve mobility of the pure gold in casting process, cobalt element peomotes Au4Dy and separates out forming core；Hardness the invention enables pure gold respectively reaches 69.3Hv and more than 105.1HV under as cast condition and aged, meets the selection of all kinds of jewellery materials.
Description
Technical field
The present invention relates to pure gold microalloy hardening technique field, a kind of hard pure gold opening-supplementing material and its system are specifically disclosed
Preparation Method.
Background technology
Currently, pure gold ornaments are still first choice of the compatriots in jewellery market, and the dosage of pure gold also occupies master in jewellery market
Lead status.The mechanical performance performance of common pure gold is softer, and solid gold jewelry easily wears or deforms, weaken jewellery appearance,
Brightness.In jewelry diamond etc. inlays class jewellery, pure gold is also commonly used as bracket material, and the weakness of mechanical property often leads to inlay
Bore or jewel comes off.Therefore, on the premise of pure gold quality is ensured, the hardness of pure gold is improved, while take into account pure gold ornaments system
Mobility, processing performance in standby process etc., are the active demands of ornaments processing market.
More mature hard pure gold ornaments are called " 3D is firmly golden " currently on the market, by galvanoplastics, can be received
Stratiform existing for metrical scale crystallite dimension is firmly golden, and refined crystalline strengthening effect is extremely prominent so that the material is keeping the same of high-purity
When there is very high hardness.But electroforming process can only process thin-walled ornaments part, the free degree of Jewelry Design is limited.And
And this nanocrystal energy is high, and grain coarsening is easy to cause under weld heating so that ornaments hardness drastically declines, and loses
Go hardening effect." 3D is firmly golden " processing technology further relates to the electrolytic solution of gold, the cyanide of severe toxicity is often used, to environment
Cause strong influence.
By V-N steel technology, it is ideal schedule of reinforcement particularly to introduce the second phase, the key of the technology
It is the design of the second phase and effectively realizes the technology for hardening purpose." jewellery are used disclosed in Chinese patent 98113521.8
Superpower high purity alloys material ", proposition uses titanium, and as intensified element, it is Au to introduce second-phase strength precipitate4Ti, can be significantly
Degree improves the hardness of pure gold.But titanium elements have very active chemical attribute and higher fusion temperature in itself, it is necessary to
Its effect of the technique competence exertion of the high melting of input price, process equipment and setting precision is wanted, therefore in traditional jewellery
Popularization in processing industry runs into very big difficulty, it is difficult to promotes on a large scale.
The content of the invention
It is an object of the invention to overcome the defects of existing, there is provided a kind of hard pure gold opening-supplementing material and preparation method thereof,
The hard pure gold opening-supplementing material can improve pure gold comprehensive mechanical property, and operating procedure is simple, reduce production cost.
In order to realize the above object the present invention is by realizing including following technical scheme：A kind of opening-supplementing material, including such as
Lower component and percentage by weight：Dysprosium 60%~85%, indium 10%~15%, zinc 0.5%~10%, cobalt 2%~10%；The dysprosium
Weight proportion with two kinds of elements of indium is 85:15.The present invention is using dysprosium doping as main intensified element, it second
Phase hardening thing is Au4Dy, and pure gold can be improved in casting process by the fusion temperature that can reduce dysprosium, addition zinc using phosphide element
In mobility；Cobalt element does not dissolve in pure gold melt, is another assisted and strengthened phase, its ambient stress field peomotes
Au4The precipitation forming core of Dy.
Preferably, which is made of following component and percentage by weight：Dysprosium 80%~85%, indium 13%~
15%th, zinc 0.5%~10%, cobalt 2%~10%.
Preferably, the weight proportion of the dysprosium and two kinds of elements of indium is 84.5~85.5:14.5~15.5.
It is highly preferred that the weight proportion of the dysprosium and two kinds of elements of indium is 85：15.The weight proportion enables to altogether
The fusing point of peritectic alloy is minimum, and Smelting Effect is best.
The present invention discloses a kind of method for preparing opening-supplementing material described above, comprises the following steps：1) protected in inert atmosphere
Under shield, the dysprosium and the indium are weighed according to part by weight, is added to carrying out melting in smelting furnace；2) dysprosium and the indium are treated
After being completely melt, the zinc and the cobalt are sequentially added, and Vibratory Mixing is uniform；3) cast it is blocking, be subsequently processed into silk material or
Particle.
Preferably, the cobalt is powdered.Cobalt element is added with powder morphology in the present invention, also act as nucleating agent effect from
And significantly crystal grain thinning, improve pure gold comprehensive mechanical property.
Preferably, the temperature of melting is 1400 DEG C~1500 DEG C in the step 1).
Preferably, in the step 2) after the dysprosium and the indium are completely melt, melt temperature is reduced to 1100 DEG C
~1250 DEG C, sequentially add the zinc and the cobalt.
The present invention discloses a kind of preparation method of hard pure gold, comprises the following steps：1) by opening-supplementing material described above with
Proof gold of the purity not less than 99.9% is 1 by weight:100 carry out dispensing, and melting is carried out using smelting technology, obtain hard foot
Gold；2) the hard pure gold is subjected to ageing treatment.
Preferably, the temperature of the melting in the step 1) is 1150 DEG C~1200 DEG C.
Preferably, the hardness of the step 1) acquisition hard pure gold reaches more than 69.3Hv.
Preferably, the temperature of ageing treatment described in the step 2) is 450 DEG C~600 DEG C.
Preferably, the time of ageing treatment described in the step 2) is 0.5-3h.
Preferably, in the step 2), the hardness of the hard pure gold reaches more than 105.1Hv after ageing treatment.
Invention additionally discloses hard pure gold prepared by a kind of method described above.
In conclusion the present invention provides a kind of hard pure gold opening-supplementing material and preparation method thereof, beneficial effects of the present invention：
For the present invention using dysprosium doping as main intensified element, its second phase hardening thing is Au4Dy.Use phosphide element
Collocation can reduce the fusion temperature of dysprosium in proportion, it is ensured that it adapts to conventional noble metal jewelry smelting technology.Adding zinc can
To improve mobility of the pure gold in casting process.Cobalt element does not dissolve in pure gold melt, is another assisted and strengthened phase, around it
Stress field peomotes the precipitation forming core of Au4Dy.Cobalt element is added with powder morphology in the present invention at the same time, also acts as nucleating agent
Effect, so that significantly crystal grain thinning, improves pure gold comprehensive mechanical property.The hard pure gold of the present invention is in as cast condition and aged
Lower hardness respectively reaches 69.3Hv and more than 105.1HV, meets the selection of all kinds of jewellery materials.
Embodiment
With reference to embodiment, the present invention is further explained.It is to be understood that embodiment is merely to illustrate the present invention, and it is unrestricted
The scope of the present invention.
Embodiment 1
Opening-supplementing material is prepared first, by weight progress dispensing, dysprosium 75.0%, indium 13.2%, zinc 3.5%, cobalt powder 8.3%
Cobalt powder average diameter is 2mm.Two kinds of metals of dysprosium and indium are placed in graphite crucible, spelter and cobalt powder are divided to two lattice to be individually positioned in stove
In top interlayer, which can pour into charging by exterior Mechanical course.5*10 is evacuated to after closing fire door-3Pa, is then charged with argon
Gas, air pressure are 0.8 atmospheric pressure.Melting dysprosium-indium bianry alloy, fusion temperature reach 1450 in proportion under inert atmosphere protection
DEG C it is completely melt bianry alloy, then descends adjusting power that melt temperature is reduced to 1150 DEG C, sequentially add spelter and cobalt rapidly
Powder, and Vibratory Mixing is carried out to crucible, it is cast in the mould being pre-placed, obtains pure gold opening-supplementing material.In order to which dispensing is convenient,
Pure gold opening-supplementing material is cut into fritter, facilitates dispensing.
The proof gold of pure gold opening-supplementing material and purity not less than 99.9% is pressed 1:100 ratio dispensings, are melted using peace well equipment
Refining obtains hard pure gold, and fusion temperature is 1200 DEG C, obtains as cast condition hard pure gold sample.Cut portion hard pure gold sample exists
When 500 DEG C of progress ageing treatments 1 are small, aged hard pure gold sample is obtained.
The hard pure gold sample of as cast condition hard pure gold sample and aged is respectively cut, carries out hardness test.
Embodiment 2
Opening-supplementing material is prepared first, by weight progress dispensing, dysprosium 80.0%, indium 14.1%, spelter 2.0%, cobalt powder
3.9%, cobalt powder average diameter is 1mm.Two kinds of metals of dysprosium and indium are placed in graphite crucible, spelter and cobalt powder are divided to two lattice to put respectively
Put in furnace roof interlayer.3*10 is evacuated to after closing fire door-3Pa, is then charged with argon gas, and air pressure is 0.8 atmospheric pressure.Lazy
Melting dysprosium-indium bianry alloy in proportion under property atmosphere protection, fusion temperature, which reaches 1400 DEG C, is completely melt bianry alloy, then
Lower adjusting power melt temperature is reduced to 1200 DEG C, sequentially adds spelter and cobalt powder rapidly, and Vibratory Mixing, casting are carried out to crucible
Into the mould being pre-placed, pure gold opening-supplementing material is obtained.Pure gold opening-supplementing material tabletting is cut into fritter, facilitates dispensing.
Second step melting hard pure gold, 1 is pressed by the pure gold opening-supplementing material and purity not less than 99.9% proof gold:100 ratios
Dispensing, obtains hard pure gold, fusion temperature is 1200 DEG C, obtains as cast condition hard pure gold sample using peace well equipment melting.Cutting
Part hard pure gold sample carries out ageing treatment 40 minutes at 550 DEG C, obtains aged hard pure gold sample.
The hard pure gold sample of as cast condition hard pure gold sample and aged is respectively cut, carries out hardness test.
Embodiment 3
Opening-supplementing material is prepared first, by weight progress dispensing, dysprosium 70.0%, indium 12.4%, spelter 9.0%, cobalt powder
8.6%, cobalt powder average diameter is 20mm.Two kinds of metals of dysprosium and indium are placed in graphite crucible, spelter and cobalt powder are divided to two lattice to distinguish
It is placed in furnace roof interlayer.5*10 is evacuated to after closing fire door-3Pa, is then charged with argon gas, and air pressure is 0.8 atmospheric pressure.
Melting dysprosium-indium bianry alloy in proportion under inert atmosphere protection, fusion temperature, which reaches 1480 DEG C, is completely melt bianry alloy, so
Descend adjusting power to reduce melt temperature to 1120 DEG C afterwards, sequentially add spelter and cobalt powder rapidly, and Vibratory Mixing is carried out to crucible, pour
Cast onto in the mould being pre-placed, obtain pure gold opening-supplementing material.Opening-supplementing material tabletting is cut into fritter, facilitates dispensing.
Second step melting hard pure gold, 1 is pressed by the opening-supplementing material and purity not less than 99.9% proof gold:100 ratio dispensings,
Hard pure gold is obtained using conventional peace well equipment melting, fusion temperature is 1180 DEG C, obtains as cast condition hard pure gold sample.Cutting part
Divide hard pure gold sample to carry out ageing treatment 30 minutes at 600 DEG C, obtain the pure gold sample of aged hard.
As cast condition hard pure gold sample and aged hard pure gold sample is respectively cut, carries out hardness test.
Embodiment 4
Opening-supplementing material is prepared first, by weight progress dispensing, dysprosium 82.5%, indium 14.6%, spelter 0.8%, cobalt powder
2.1%, cobalt powder average diameter is 50 microns.Two kinds of metals of dysprosium and indium are placed in graphite crucible, spelter and cobalt powder are divided to two lattice point
It is not placed in furnace roof interlayer.5*10 is evacuated to after closing fire door-3Pa, is then charged with argon gas, and air pressure is 0.8 atmospheric pressure.
Melting dysprosium-indium bianry alloy under inert atmosphere protection, fusion temperature, which reaches 1450 DEG C, is completely melt bianry alloy, then under
Adjusting power reduces melt temperature to 1140 DEG C, sequentially adds spelter and cobalt powder rapidly, and carries out Vibratory Mixing to crucible, is cast to
In the mould being pre-placed, opening-supplementing material is obtained.Then opening-supplementing material tabletting is cut into fritter, facilitates dispensing.
Second step melting hard pure gold, 1 is pressed by the proof gold of the opening-supplementing material and purity not less than 99.9%:100 ratios are matched somebody with somebody
Material, obtains hard pure gold, fusion temperature is 1160 DEG C, obtains as cast condition hard pure gold sample using conventional peace well equipment melting.Cut
Part hard pure gold sample is cut when 450 DEG C of progress ageing treatments 3 are small, obtains the hard pure gold sample of aged.
Test result
Testing example 1 to 4 obtains hard pure gold sample and such as sees respectively in as cast condition and the hardness of aged, test result
Shown in Tables 1 and 2.
Hardness (unit of the hard pure gold sample that 1 embodiment 1 to 4 of table obtains in as cast condition：Hv)
Hardness (unit of the hard pure gold sample that 2 embodiment 1 to 4 of table obtains in aged：Hv)
| 1 | 2 | 3 | 4 | 5 | Average hardness | |
| Embodiment 1 | 113.9 | 117.5 | 110.8 | 114.5 | 118.6 | 115.1 |
| Embodiment 2 | 128.8 | 131.4 | 130.2 | 125.9 | 127.1 | 128.7 |
| Embodiment 3 | 106.2 | 104.7 | 107.1 | 101.8 | 105.9 | 105.1 |
| Embodiment 4 | 145.2 | 138.7 | 139.7 | 140.9 | 142.2 | 141.3 |
As it can be seen from table 1 the hard pure gold sample of present invention hardness under as cast condition has reached more than 69.3Hv, in timeliness
It is even more that can reach more than 105.1Hv after processing, improves 3 times and more than 4 times than common 24K gold respectively.These hardness refer to
Mark has reached the international advanced standard of current report, suitable for inlaying class bullion and luxury goods Watch dail plate, electronics production
Product etc. promote and apply.
To sum up, for the present invention using dysprosium doping as main intensified element, its second phase hardening thing is Au4Dy.Use
Phosphide element is arranged in pairs or groups in proportion can reduce the fusion temperature of dysprosium, it is ensured that it adapts to conventional noble metal jewelry smelting technology.Add
Zincification can improve mobility of the pure gold in casting process.Cobalt element peomotes the precipitation forming core of Au4Dy.This hair at the same time
Bright middle cobalt element is added with powder morphology, also acts as nucleating agent effect, so that significantly crystal grain thinning, improves pure gold synthesis mechanics
Performance.The hard pure gold of present invention hardness under as cast condition and aged respectively reaches 69.3Hv and more than 105.1HV, meets each
The selection of class jewellery material.So the present invention effectively overcomes various shortcoming of the prior art and has high industrial exploitation value
Value.
The above, be only presently preferred embodiments of the present invention, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, on the premise of the method for the present invention is not departed from, can also make
Some improvement and supplement, these are improved and supplement also should be regarded as protection scope of the present invention.All those skilled in the art,
Without departing from the spirit and scope of the present invention, when made using disclosed above technology contents it is a little more
Dynamic, modification and the equivalent variations developed, are the equivalent embodiment of the present invention；Meanwhile all substantial technologicals pair according to the present invention
The variation, modification and evolution for any equivalent variations that above-described embodiment is made, still fall within the scope of technical scheme
It is interior.
Claims (10)
- A kind of 1. opening-supplementing material, it is characterised in that：Including following component and percentage by weight：Dysprosium 60%~85%, indium 10%~ 15%th, zinc 0.5%~10%, cobalt 2%~10%；The weight proportion of the dysprosium and two kinds of elements of indium is 84~86:14~ 16；The opening-supplementing material is made by following preparation methods, is comprised the following steps：1) under inert atmosphere protection, the dysprosium and the indium are weighed according to percentage by weight, is added to being melted in smelting furnace Refining；2) after the dysprosium and the indium are completely melt, the zinc and the cobalt are sequentially added, and Vibratory Mixing is uniform；3) cast blocking, be subsequently processed into silk material or particle；The cobalt is powdered.
- 2. opening-supplementing material as claimed in claim 1, it is characterised in that：The weight proportion of the dysprosium and two kinds of elements of indium is 84.5~85.5:14.5~15.5.
- A kind of 3. method for preparing opening-supplementing material as claimed in claim 1 or 2, it is characterised in that：Comprise the following steps：1) under inert atmosphere protection, the dysprosium and the indium are weighed according to percentage by weight, is added to being melted in smelting furnace Refining；2) after the dysprosium and the indium are completely melt, the zinc and the cobalt are sequentially added, and Vibratory Mixing is uniform；3) cast blocking, be subsequently processed into silk material or particle.
- 4. the preparation method of opening-supplementing material as claimed in claim 3, it is characterised in that：The cobalt is powdered.
- 5. the preparation method of opening-supplementing material as claimed in claim 3, it is characterised in that：The temperature of melting in the step 1) For 1400 DEG C~1500 DEG C.
- 6. the preparation method of opening-supplementing material as claimed in claim 3, it is characterised in that：Treated in the step 2) dysprosium and After the indium is completely melt, melt temperature is reduced to 1100 DEG C~1250 DEG C, sequentially adds the zinc and the cobalt.
- 7. a kind of preparation method of hard pure gold, it is characterised in that comprise the following steps：1) it is 1 by weight by the proof gold of opening-supplementing material as claimed in claim 1 or 2 and purity not less than 99.9%:100 into Row dispensing, carries out melting using smelting technology, obtains hard pure gold；2) the hard pure gold is subjected to ageing treatment.
- 8. the preparation method of hard pure gold as claimed in claim 7, it is characterised in that the melting in the step 1) Temperature is 1150 DEG C~1200 DEG C.
- 9. the preparation method of hard pure gold as claimed in claim 7, it is characterised in that ageing treatment described in the step 2) Temperature is 450 DEG C~600 DEG C；And/or aging time described in the step 2) is 0.5-3h.
- A kind of 10. hard pure gold prepared by any method of claim 7 to 9.
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| CN110699586B (en) * | 2019-11-21 | 2020-09-18 | 山东省计量科学研究院 | Hard pure silver joint coating material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921925A (en) * | 2010-09-08 | 2010-12-22 | 深圳市金福珠宝首饰有限公司 | Gold alloy and preparation method thereof |
| CN102127659A (en) * | 2011-01-13 | 2011-07-20 | 上海交通大学 | Method for optimizing strength of thousand pure gold jewellery and gold alloy material |
| CN102676864A (en) * | 2012-06-06 | 2012-09-19 | 广东潮宏基实业股份有限公司 | Formula and preparation method of purple K gold |
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| JP2009068058A (en) * | 2007-09-12 | 2009-04-02 | Citizen Holdings Co Ltd | Decorative parts |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921925A (en) * | 2010-09-08 | 2010-12-22 | 深圳市金福珠宝首饰有限公司 | Gold alloy and preparation method thereof |
| CN102127659A (en) * | 2011-01-13 | 2011-07-20 | 上海交通大学 | Method for optimizing strength of thousand pure gold jewellery and gold alloy material |
| CN102676864A (en) * | 2012-06-06 | 2012-09-19 | 广东潮宏基实业股份有限公司 | Formula and preparation method of purple K gold |
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