CN105087997B - A kind of red billon and preparation method thereof for firing temperature resistant transparent enamel - Google Patents
A kind of red billon and preparation method thereof for firing temperature resistant transparent enamel Download PDFInfo
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- CN105087997B CN105087997B CN201510481972.1A CN201510481972A CN105087997B CN 105087997 B CN105087997 B CN 105087997B CN 201510481972 A CN201510481972 A CN 201510481972A CN 105087997 B CN105087997 B CN 105087997B
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Abstract
The invention discloses a kind of red billons and preparation method thereof for firing temperature resistant transparent enamel.It is a kind of for firing the red billon of temperature resistant transparent enamel, it is comprised the following ingredients: 75.0-75.5wt% gold, 22.5-23.2wt% copper, 0.9-1.2wt% silver, 0.5-0.8wt% zinc, 0.2-0.4wt% palladium, 0.01-0.03wt% silicon, 0.008-0.02wt% scandium, 0.0005-0.001wt% boron and other inevitable impurity.For firing the preparation method of the red billon of temperature resistant transparent enamel, it is characterised in that: step are as follows: 1) raw material is carried out melting under protective atmosphere；2) after material is all melting down, the temperature of molten metal is adjusted, casting obtains ingot casting.Red billon of the invention has good high temperature oxidation resistance, can preferably bear high temperature firing；The thermal expansion coefficient of thermal expansion coefficient and common gold high-temperature glaze is close；With excellent cold-forming property, do not occur brittle failure phenomenon in process；Crystal grain is tiny, dense structure, help to obtain press polished surface.
Description
Technical field
The present invention relates to a kind of red billons and preparation method thereof for firing temperature resistant transparent enamel.
Background technique
In karat gold series, the red gold of K, because of the magnificent elegance of its color, becomes wind compared with the platinum of gorgeous gold and low-key
Row is in current international jewellery industry, particularly oriental trend fashion.Insider assigns this according to its unique color
One romantic name of class material, is rose gold, represents the eternal theme of the mankind --- love.Enamel technique applies to rose
On gold ornaments, the artistic effect of jewellery can be dramatically increased, but uses rose gold common on the market as firing high temperature enamel
When the substrate of thinkling sound, it is commonly encountered several distinct issues: first is that alloy material, which fires rear surface through high temperature, aoxidizes very serious, influence
The decorative effect of enamel, such as Fig. 1；Second is that the metallic substrates fired after enamel become fragile, waited in subsequent polishing, edge stone, polishing
Fracture is easy to appear in journey, alloy is easy to break just as dried firewood when embrittlement is serious, such as Fig. 2, completely not like excellent expensive of toughness plasticity
Metal alloy brings very big puzzlement and difficulty to jewellery production；Third is that rose gold ornaments is using or is placing a period of time, surface
It is easy dark and gloomy and discoloration, without initial brightness and color；Fourth is that frequently encountering surface shrinkage porosite when casting rose gold ornaments
Problem, the severe exacerbation surface quality of ornaments, such as Fig. 3.Especially when substrate fills out glaze and shrinkage porosite occurs, enamel can be seriously affected
The decorative effect of thinkling sound causes enamel layer muddy stain or explosion.When large-scale shrinkage porosite problem occur in jewellery, such as pass through welding
Or sanding and polishing processing, workload is very big, and both time-consuming, effect is again poor, only scraps gadget when many, affects enterprise
Manufacturing schedule and cost.
Summary of the invention
The purpose of the present invention is to provide a kind of red billons and preparation method thereof for firing temperature resistant transparent enamel.
The technical solution used in the present invention is:
It is a kind of for firing the red billon of temperature resistant transparent enamel, comprise the following ingredients: 75.0-75.5wt%
Gold, 22.5-23.2wt% copper, 0.9-1.2wt% silver, 0.5-0.8wt% zinc, 0.2-0.4wt% palladium, 0.01-0.03wt% silicon,
0.008-0.02wt% scandium, 0.0005-0.001wt% boron and other inevitable impurity.
It is made of the raw material of following mass percent: 1-2wt% copper scandium alloy, 5-8wt% copper palldium alloy, 0-11wt%
Yellow gold, 0-1wt% silver-colored zinc alloy, 1-3wt% cupro silicon, 0-1wt% fine silver, 4.5-11.5 wt% ormolu, 0.4-
0.5 wt% Cu-B alloy, 2-7 wt% fine copper, 75.0-75.5wt% proof gold.
In the yellow gold, silver-colored content is 5wt%.
In the copper palldium alloy, the content of palladium is 5wt%.
In the copper scandium alloy, the content of scandium is 1wt%.
In the cupro silicon, the content of silicon is 1wt%；In silver-colored zinc alloy, the content of zinc is 30wt%.
The preparation method of the red billon for firing temperature resistant transparent enamel, step are as follows:
1) raw material is subjected to melting under protective atmosphere；
2) after material is all melting down, the temperature of molten metal is adjusted, casting obtains ingot casting；
3) it by after ingot casting roll compacting, anneals.
In step 1), the protective atmosphere is industrial straight argon.
In step 1), melting is carried out in induction furnace, smelting temperature is 1020-1040 DEG C.
In step 2, the temperature of molten metal is adjusted to 1010-1030 DEG C.
The beneficial effects of the present invention are:
(1) red billon of the invention has good high temperature oxidation resistance, can preferably bear high temperature firing,
The transparent enamel layer fired has good bright degree, and crystal grain is not grown up after firing repeatedly for several times.
(2) thermal expansion coefficient of the thermal expansion coefficient of red billon of the invention and common gold high-temperature glaze is close,
Keep the enamel layer after firing relatively stable, is less prone to the problems such as explosion is peeled off.
(3) red billon of the invention has excellent cold-forming property, does not occur brittle failure phenomenon in process.
(4) red billon crystal grain of the invention is tiny, and dense structure help to obtain press polished surface.
Detailed description of the invention
Fig. 1 is the pictorial diagram of severe oxidation when commercially available 18K rose gold fires enamel；
Fig. 2 is to occur the pictorial diagram of brittle failure during the grinding process after commercially available 18K rose gold fires enamel；
Fig. 3 is the pictorial diagram of commercially available 18K rose gold surface shrinkage porosite；
Fig. 4 is the microscopic structure (300 ×) of 18K red billon of the present invention；
Fig. 5 is polarization curve of the 18K red billon of the present invention in 37 DEG C of synthetic perspirations；
Fig. 6 is that 18K red billon of the present invention impregnates the reflectance curve after 1 hour in sodium sulfide solution；
Fig. 7 is the oxidation after 18K red billon of the present invention and commercially available 18K red billon heat 1.5 hours at 750 DEG C
Film situation comparison diagram (200 ×)；
Fig. 8 is the temperature thermal dilatometry of 18K red billon of the present invention；
Fig. 9 is the cold work hardening curve of 18K red billon of the present invention.
Specific embodiment
It is a kind of for firing the red billon of temperature resistant transparent enamel, comprise the following ingredients: 75.0-75.5wt%
Gold, 22.5-23.2wt% copper, 0.9-1.2wt% silver, 0.5-0.8wt% zinc, 0.2-0.4wt% palladium, 0.01-0.03wt% silicon,
0.008-0.02wt% scandium, 0.0005-0.001wt% boron and other inevitable impurity.
It is made of the raw material of following mass percent: 1-2wt% copper scandium alloy, 5-8wt% copper palldium alloy, 0-11wt%
Yellow gold, 0-1wt% silver-colored zinc alloy, 1-3wt% cupro silicon, 0-1wt% fine silver, 4.5-11.5 wt% ormolu, 0.4-
0.5 wt% Cu-B alloy, 2-7 wt% fine copper, 75.0-75.5wt% proof gold.
Preferably, in raw material used in (including embodiment) of the invention: in the yellow gold, silver-colored content is
5wt%；In the copper palldium alloy, the content of palladium is 5wt%；In the copper scandium alloy, the content of scandium is 1wt%；The copper
In silicon alloy, the content of silicon is 1wt%；In silver-colored zinc alloy, the content of zinc is 30wt%.
The preparation method of the red billon for firing temperature resistant transparent enamel, step are as follows:
1) raw material is subjected to melting under protective atmosphere；
2) after material is all melting down, the temperature of molten metal is adjusted, casting obtains ingot casting；
3) it by after ingot casting roll compacting, anneals.
Preferably, in step 1), the protective atmosphere is industrial straight argon.
Preferably, step 1) are as follows: proof gold is rolled into thin slice, wraps up silver-colored scandium alloy, silver palladium alloy, yellow gold, copper with it
Kirsite, cupro silicon, fine silver, are put into graphite crucible, carry out melting, smelting temperature using induction heating under protective atmosphere
It is 1020-1040 DEG C；
Preferably, in step 2, the temperature of molten metal is adjusted to 1010-1030 DEG C.
Preferably, it makes annealing treatment are as follows: anneal 3-10 minutes at 700-800 DEG C.
The present invention is described further combined with specific embodiments below:
Embodiment 1:
The red billon for being used to fire high temperature enamel of the present embodiment, is made of following ingredients by mass percentage:
75.20wt% gold, 22.87wt% copper, 1.07wt% silver, 0.53wt% zinc, 0.30wt% palladium, 0.015wt% silicon,
0.013wt% scandium, 0.0008wt% boron and other inevitable impurity.
The preparation method of the present embodiment the following steps are included:
Melting is carried out in vaccum sensitive stove, the mass percent of the raw material is respectively as follows: 1.3wt% copper scandium alloy, 6wt%
Copper palldium alloy, 7.3wt% Kufil, 1.5wt% cupro silicon, 0.7wt% fine silver, 7.6wt% ormolu, 0.4wt% copper boron close
Gold, 75.2wt% proof gold.Above-mentioned material is sequentially placed into graphite crucible, fill closely knit and closes bell, is evacuated down to 4.4Pa,
Industrial straight argon is filled with to 1.01atm.Start induction heating and carry out melting, smelting temperature is 1030-1040 DEG C.Furnace charge is all melting down
Afterwards, adjustment molten metal temperature is 1020-1030 DEG C, and ingot casting will be made in pouring metal melt to ingot mould.After ingot casting roll compacting,
750 DEG C are annealed 5 minutes.
18K red billon made from the present embodiment does not occur apparent shrinkage defect, annealed state microscopic structure such as Fig. 4,
Alloy structure is fine and close tiny equiax crystal, this is conducive to the strength character and polishing performance of material.
Priming color the coordinate value L*, a*, b* of 18K red billon made from the present embodiment are respectively 85.93,9.94 Hes
16.21, in the red billon region of color area figure, show as good red.This implementation alloy is in 37 DEG C of synthetic perspirations
In polarization behavior such as Fig. 5, apparent passivation has occurred during electric potential scanning, causes blunt current potential higher alloy.Alloy is hanged
Hang the sodium sulfide solution progress corrosion test for being immersed in that concentration is 5%, temperature is 30 DEG C, after etch 1 hour, its opposite initial face
Color seems partially red partially yellow, and it is poor not show naked eyes perceived color by brightness decline, the not apparent variation of reflectivity, such as Fig. 6
Not, show that alloy has preferable corrosion resisting property and discoloration-resisting.
18K red billon made from the present embodiment and commercially available 18K red billon are after 750 DEG C are heated 1.5 hours
Oxidation film situation comparison such as Fig. 7, the oxidation film layer of alloy of the present invention is very thin, compact structure, plays the role of being effectively protected, and prevents
Interior metal continues to aoxidize, and embodies preferable high temperature oxidation resistance, and the oxidation film layer of commercial alloys obviously compares the present invention
Alloy wants thick.
The fusion temperature range of 18K red billon of the present invention is 905-918 DEG C, can preferably bear the firing temperature of enamel
Degree.It is that the temperature thermal dilatometry of alloy is as shown in figure 8, warm with common golden high temperature glaze between 38-828 DEG C in temperature
The coefficient of expansion is close, thus is conducive to the combination of glassy surface and substrate, it is not easy to the problems such as bursting or peeling off occurs.
18K red billon annealed state hardness made from the present embodiment is HV185, and curve such as Fig. 9 is cold worked, shows good
Good processing performance, does not occur brittle failure phenomenon.
The transparency of transparent enamel set jewelry of the 18K red billon of the present invention as substrate fabrication, enamel layer is high, base
The clean mark at bottom is as it can be seen that bubble is few, and the combination of substrate is stablized, and the jewel inlayed is secured.
Embodiment 2:
The red billon for being used to fire high temperature enamel of the present embodiment, is made of following ingredients by mass percentage:
75.0wt% gold, 1.13wt% silver, 23.06wt% copper, 0.51wt% zinc, 0.26wt% palladium, 0.028wt% silicon,
0.020wt% scandium, 0.0010wt% boron and other inevitable impurity.
The preparation method of the present embodiment the following steps are included:
Melting is carried out in vaccum sensitive stove, the mass percent of the raw material is respectively as follows: 2wt% copper scandium alloy, 5.1wt%
Copper palldium alloy, 6.5wt% Kufil, 2.8wt% cupro silicon, 0.8wt% fine silver, 7.3wt% ormolu, 0.5wt% copper boron close
Gold, 75.0wt% proof gold.Above-mentioned material is sequentially placed into graphite crucible, fill closely knit and closes bell, is evacuated down to 4.7Pa,
Industrial straight argon is filled with to 1.02atm.Start induction heating and carry out melting, smelting temperature is 1020-1030 DEG C.Furnace charge is all melting down
Afterwards, adjustment molten metal temperature is 1010-1020 DEG C, and ingot casting will be made in pouring metal melt to ingot mould.After ingot casting roll compacting,
750 DEG C are annealed 5 minutes.
Embodiment 3:
The red billon for being used to fire high temperature enamel of the present embodiment, is made of following ingredients by mass percentage:
75.5wt% gold, 0.90wt% silver, 22.64wt% copper, 0.60wt% zinc, 0.30wt% palladium, 0.030wt% silicon,
0.016wt% scandium, 0.0010wt% boron and other inevitable impurity.
The preparation method of the present embodiment the following steps are included:
Melting is carried out in vaccum sensitive stove, the mass percent of the raw material is respectively as follows: 1.6wt% copper scandium alloy, 6wt%
Copper palldium alloy, 4wt% Kufil, 3wt% cupro silicon, 0.7wt% fine silver, 8.7wt% ormolu, 0.5wt% Cu-B alloy,
75.5wt% proof gold.Above-mentioned material is sequentially placed into graphite crucible, fill closely knit and closes bell, 4.8Pa is evacuated down to, fills
Enter industrial straight argon to 1.0atm.Start induction heating and carry out melting, smelting temperature is 1030-1040 DEG C.After furnace charge is all melting down,
Adjusting molten metal temperature is 1020-1030 DEG C, and ingot casting will be made in pouring metal melt to ingot mould.After ingot casting roll compacting, 750
DEG C annealing 5 minutes.
Embodiment 4:
The red billon for being used to fire high temperature enamel of the present embodiment, is made of following ingredients by mass percentage:
75.10wt% gold, 0.97wt% silver, 23.18wt% copper, 0.50wt% zinc, 0.20wt% palladium, 0.027wt% silicon,
0.015wt% scandium, 0.0008wt% boron and other inevitable impurity.
The preparation method of the present embodiment the following steps are included:
Melting is carried out in vaccum sensitive stove, the mass percent of the raw material is respectively as follows: 1.5wt% copper scandium alloy, 4wt%
Copper palldium alloy, 11wt% Kufil, 0.6 wt% silver-colored zinc alloy, 2.7wt% cupro silicon, 4.7wt% ormolu, 0.4wt% copper
Boron alloy, 75.1wt% proof gold.Above-mentioned material is sequentially placed into graphite crucible, fill closely knit and closes bell, is evacuated down to
4.6Pa is filled with industrial straight argon to 0.99atm.Start induction heating and carry out melting, smelting temperature is 1020-1030 DEG C.Furnace charge is complete
After portion is melting down, adjustment molten metal temperature is 1010-1020 DEG C, and ingot casting will be made in pouring metal melt to ingot mould.Ingot casting is rolled
After pressure, anneal 5 minutes at 750 DEG C.
Embodiment 5:
The red billon for being used to fire high temperature enamel of the present embodiment, is made of following ingredients by mass percentage:
75.40wt% gold, 0.90wt% silver, 22.51wt% copper, 0.78wt% zinc, 0.39wt% palladium, 0.010wt% silicon,
0.011wt% scandium, 0.0008wt% boron and other inevitable impurity.
The preparation method of the present embodiment the following steps are included:
Melting is carried out in vaccum sensitive stove, the mass percent of the raw material is respectively as follows: 1.1wt% copper scandium alloy,
7.7wt% copper palldium alloy, 1wt% cupro silicon, 0.9wt% fine silver, 11.2wt% ormolu, 0.4wt% Cu-B alloy, 2.3 wt%
Fine copper, 75.4wt% proof gold.Above-mentioned material is sequentially placed into graphite crucible, fill closely knit and closes bell, is evacuated down to
5.0Pa is filled with industrial straight argon to 1.0atm.Start induction heating and carry out melting, smelting temperature is 1030-1040 DEG C.Furnace charge is complete
After portion is melting down, adjustment molten metal temperature is 1020-1030 DEG C, and ingot casting will be made in pouring metal melt to ingot mould.Ingot casting is rolled
After pressure, anneal 5 minutes at 750 DEG C.
Embodiment 6:
The red billon for being used to fire high temperature enamel of the present embodiment, is made of following ingredients by mass percentage:
75.30wt% gold, 0.95wt% silver, 22.92wt% copper, 0.55wt% zinc, 0.25wt% palladium, 0.014wt% silicon,
0.010wt% scandium, 0.0010wt% boron and other inevitable impurity.
The preparation method of the present embodiment the following steps are included:
Melting is carried out in vaccum sensitive stove, the mass percent of the raw material is respectively as follows: 1wt% copper scandium alloy, 5wt% copper
Palldium alloy, 1wt% Kufil, 1.4wt% cupro silicon, 0.9wt% fine silver, 8wt% ormolu, 0.5wt% Cu-B alloy,
6.9wt% fine copper, 75.3wt% proof gold.Above-mentioned material is sequentially placed into graphite crucible, fill closely knit and closes bell, is vacuumized
To 4.8Pa, industrial straight argon is filled with to 1.0atm.Start induction heating and carry out melting, smelting temperature is 1020-1030 DEG C.Furnace charge
After whole is melting down, adjustment molten metal temperature is 1010-1020 DEG C, and ingot casting will be made in pouring metal melt to ingot mould.By ingot casting
After roll compacting, anneal 5 minutes at 750 DEG C.
Claims (10)
1. a kind of for firing the red billon of temperature resistant transparent enamel, it is characterised in that: it is comprised the following ingredients:
75.0-75.5wt% gold, 22.5-23.2wt% copper, 0.9-1.2wt% silver, 0.5-0.8wt% zinc, 0.2-0.4wt% palladium, 0.01-
0.03wt% silicon, 0.008-0.02wt% scandium, 0.0005-0.001wt% boron and other inevitable impurity.
2. according to claim 1 a kind of for firing the red billon of temperature resistant transparent enamel, it is characterised in that: it is
It is made of the raw material of following mass percent: 1-2wt% copper scandium alloy, 5-8wt% copper palldium alloy, 0-11wt% yellow gold, 0-
1wt% silver-colored zinc alloy, 1-3wt% cupro silicon, 0-1wt% fine silver, 4.5-11.5 wt% ormolu, 0.4-0.5 wt% copper boron close
Gold, 2-7 wt% fine copper, 75.0-75.5wt% proof gold.
3. according to claim 2 a kind of for firing the red billon of temperature resistant transparent enamel, it is characterised in that: described
Yellow gold in, silver-colored content be 5wt%.
4. according to claim 2 a kind of for firing the red billon of temperature resistant transparent enamel, it is characterised in that: described
Copper palldium alloy in, the content of palladium is 5wt%.
5. according to claim 2 a kind of for firing the red billon of temperature resistant transparent enamel, it is characterised in that: described
Copper scandium alloy in, the content of scandium is 1wt%.
6. according to claim 2 a kind of for firing the red billon of temperature resistant transparent enamel, it is characterised in that: described
Cupro silicon in, the content of silicon is 1wt%；In silver-colored zinc alloy, the content of zinc is 30wt%.
7. it is of any of claims 1-6 for firing the preparation method of the red billon of temperature resistant transparent enamel,
It is characterized in that: step are as follows:
1) raw material is subjected to melting under protective atmosphere；
2) after material is all melting down, the temperature of molten metal is adjusted, casting obtains ingot casting；
3) it by after ingot casting roll compacting, anneals.
8. according to claim 7 for firing the preparation method of the red billon of temperature resistant transparent enamel, feature exists
In: in step 1), the protective atmosphere is industrial straight argon.
9. according to claim 7 for firing the preparation method of the red billon of temperature resistant transparent enamel, feature exists
In: in step 1), melting is carried out in induction furnace, smelting temperature is 1020-1040 DEG C.
10. according to claim 7 for firing the preparation method of the red billon of temperature resistant transparent enamel, feature exists
In: in step 2, the temperature of molten metal is adjusted to 1010-1030 DEG C.
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