CN1036234A - Black cubic zirconia jewel and manufacture method thereof - Google Patents
Black cubic zirconia jewel and manufacture method thereof Download PDFInfo
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- CN1036234A CN1036234A CN 89102170 CN89102170A CN1036234A CN 1036234 A CN1036234 A CN 1036234A CN 89102170 CN89102170 CN 89102170 CN 89102170 A CN89102170 A CN 89102170A CN 1036234 A CN1036234 A CN 1036234A
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- black
- jewel
- cubic
- cubic zirconia
- zirconium oxide
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Abstract
The invention relates to the technology of black cubic zirconia jewel and method for making thereof, it discloses the processing condition that adopt thermal treatment cubic crystal of zirconium oxide under vacuum condition or reducing atmosphere or the inert atmosphere, prepares the black cubic zirconia jewel that can not obtain by adulterating method.
Description
The invention relates to the manufacture method of black cubic crystal of zirconium oxide and the technology of black cubic zirconia gem products.
About the early existing many documents and materials reports of the manufacturing technology of cubic crystal of zirconium oxide, as U.S.P.N
O4153469, GBP N
O1491362 etc., adopt " cold crucible " method, according to following prescription: ZrO
370～95 weight percentage, Y
2O
330～5 weight percentage, the oxide compound 0～5% of all the other coloring elements, melting under the condition of ratio-frequency heating, cooling obtain cubic crystal of zirconium oxide.Yet the black cubic crystal of zirconium oxide is not seen the document announcement that product and method for making are arranged so far as yet.
Black also is the necessary color in the life, in order to decorate people's life, increases living color, and the cubic zirconia jewel of development black necessitates.Yet by in melting, adding the relevant transition metal oxide or the painted means of rare-earth oxide, do not obtain to be complete black cubic crystal of zirconium oxide all the time, therefore, taked the crystalline post-processing technology to realize this purpose.
(Gao Haiqing translates " thermal treatment of diamond material ", " jewel ", first phase P73～79 in 1987, Beijing jewel institute) principle and method that some jewel thermal treatment color and lusters change have been introduced, and the formation of pointing out oxygen room in the crystalline structure will cause the variation of color and luster, though do not relate to the problem of cubic zirconia, given us useful enlightenment.We have analyzed the The Nomenclature Composition and Structure of Complexes state of cubic zirconia, and thinking has ready conditions causes the oxygen room of cubic zirconia, and the oxygen room is increased, thereby form the point defect with the heart, have produced the absorption effect to light.Stable cubic crystal of zirconium oxide, Y
2O
3Be stablizer, Y in the cubic system structure
2O
3Introducing, produced certain oxygen room, Y in structure
3+Occupied Zr
4+Some position, two Y of every introducing
3+Ion just produces an O
2-The room forms colour center down behind the trapped electron of this room.Since after producing the oxygen room, O
2-The ionic activity has increased, and can move in limited range, if create conditions suitable, increases O
2-Energy, make O in the crystal
2-Be reduced into O
2Oxygen is emitted, and increases oxygen room in the structure, produces more F colour center point defect, and light absorbing effect is significantly increased, and reaches the hypersorption to visible light, and cubic zirconia at this moment just becomes black.
Increase in the crystals point defect realizes by thermal treatment.Aftertreatment to cubic crystal of zirconium oxide is under vacuum condition or in reducing atmosphere or at N
2Carry out heat treated in gas, the inert atmosphere, the heat treated under this condition of process makes the O in the cubic zirconia
2Reduce, produces many F colour center point defects, make it to become black zirconia, though former water white before this cubic zirconia, still owing to having added the cubic zirconia that cubic zirconia that coloring ion formed other color can be processed into black.The present invention has special meaning to the unsafty cubic crystal of zirconium oxide of color and luster especially.After method processing of the present invention, completely all can be transformed into has the black of use value cubic zirconia.
Vacuum condition, or reducing atmosphere, or inert atmosphere, purpose all is to reduce the oxygen partial pressure of thermal treatment system, the more little effusion that just helps the oxygen in the cubic crystal of zirconium oxide structure more of system for handling oxygen partial pressure, form the oxygen room, produce F colour center point defect, help the formation of black cubic crystal of zirconium oxide.More above-mentioned condition, vacuum state are more satisfactory, and vacuum state specifically is meant certain vacuum tightness, say in principle, and vacuum tightness is high more good more, but vacuum tightness is high more, and processing cost is just high more, and through practice, vacuum tightness is 5 * 10
-3The condition of torr is just much of that.Reducing atmosphere or inert atmosphere also can cause O in the crystal
2The condition that reduces, but the pressure of system is not as vacuum state, to O
2It is not really favourable to overflow, and has only the thermal treatment temp of raising or lengthening heat treatment time to realize.
Heat treated purpose is to be to provide energy to the oxonium ion in the cubic zirconia crystallization, and enough energy are provided, and makes O
2-Enough activity are arranged, just may emit two electronics, pass the crystal barrier, formation oxygen is overflowed, in heat-processed, no matter be that intensification or cooling all must be controlled certain speed, to avoid the increasing crystalline internal stress, cause crystalline to break, influence processing characteristics and crystal intensity.
Concrete handling procedure is: the cubic crystal of zirconium oxide that desire is handled is put into the thermal treatment system and is evacuated to 5 * 10
-3The vacuum tightness that torr is above, the energising heating, speed with 100 ℃～400 ℃/hr heats up, the top temperature of heating is at 1600 ℃, at least be incubated two hours at the top temperature place, cooling then, cooling rate is 100 ℃～400 ℃/hr, in whole heat treatment process, all should keep vacuum condition, before being cooled to 600 ℃, keep vacuum condition at least.Be heat treated two examples below:
Example 1:
The water white cubic crystal of zirconium oxide of 5kg is put into heat treated vacuum systems, be evacuated to 5 * 10
-3The vacuum tightness of torr, begin heating then, be warming up to 200 ℃ with 100 ℃ speed per hour, be warming up to 1000 ℃ with 200 ℃/hr speed again, be warming up to 1700 ℃ with 400/hr speed again, under this temperature, kept two hours, be cooled to 800 ℃ and disconnected heating with 200 ℃/hr speed then, keeping under the vacuum condition, be cooled to room temperature, acquisition black cubic crystal of zirconium oxide with the rate of cooling of stove itself.
Example 2: with 5kg raggle-taggle cubic crystal of zirconium oxide, place the vacuum heat treatment system, be evacuated to 5 * 10
-3The vacuum tightness of torr, the energising heating is warming up to 300 ℃ with 100 ℃/hr speed, is warming up to 1000 ℃ with 200 ℃/hr speed again, is warming up to 1800 ℃ with 300 ℃/hr then, keeps 2.5 hours under this temperature, by the programmed cooling of example 1, obtains black crystals.
The black cubic crystal of zirconium oxide that obtains, its various physical parameters and other cubic zirconia are basically identical, and such as density, hardness, wearability etc., its unique characteristics are that crystal is black. Utilize this black cubic zirconia jewel can process and the life decoration jewel bead of pondering into various shapes, profile.
Claims (4)
1, a kind of manufacture method of black cubic crystal of zirconium oxide, to adopt the cubic crystal of zirconium oxide of the various compositions that " cold crucible " method produces to carry out aftertreatment, it is characterized in that treatment condition are to heat under vacuum condition or in reducing atmosphere or in the inert atmosphere.
2,, it is characterized in that said vacuum condition is 5 * 10 at least according to the method for claim 1 defined
-3Torr, and keep this vacuum condition in whole heat treatment process should remain at least and is cooled to below 600 ℃.
3, according to the method for claim 1 or 2 defineds, it is characterized in that said heating, top temperature is more than 1600 ℃, and intensification and cooling rate keep more than two hours at 100 ℃～400 ℃/hr at the top temperature place.
4, a kind of black cubic zirconia jewel of making according to the method for claim 1 defined, chemical constitution is: ZrO
270-95% Y
2O
330-5%, other coloring element oxide compound 0-5% can process and ponder, produces the ornament of different shape, profile, it is characterized in that this cubic zirconia jewel is a black.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89102170 CN1009285B (en) | 1989-04-15 | 1989-04-15 | Black cubic zirconia jewel and manufacture method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89102170 CN1009285B (en) | 1989-04-15 | 1989-04-15 | Black cubic zirconia jewel and manufacture method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1036234A true CN1036234A (en) | 1989-10-11 |
| CN1009285B CN1009285B (en) | 1990-08-22 |
Family
ID=4854560
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89102170 Expired CN1009285B (en) | 1989-04-15 | 1989-04-15 | Black cubic zirconia jewel and manufacture method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1009285B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100436373C (en) * | 2006-03-03 | 2008-11-26 | 中国科学院上海硅酸盐研究所 | Zirconium oxide ceramic material of ytterbium oxide and yttrium oxide costabilize |
| CN102659401A (en) * | 2012-04-24 | 2012-09-12 | 邓湘凌 | Manufacturing method for gray zirconia ceramics |
| CN108456923A (en) * | 2018-03-27 | 2018-08-28 | 汶川县神州锆业科技有限公司 | Zirconium jewel and its production method |
| CN114059161A (en) * | 2021-06-18 | 2022-02-18 | 汶川县神州锆业科技有限公司 | Zirconium gem composition and method for changing color of zirconium gem composition |
-
1989
- 1989-04-15 CN CN 89102170 patent/CN1009285B/en not_active Expired
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100436373C (en) * | 2006-03-03 | 2008-11-26 | 中国科学院上海硅酸盐研究所 | Zirconium oxide ceramic material of ytterbium oxide and yttrium oxide costabilize |
| CN102659401A (en) * | 2012-04-24 | 2012-09-12 | 邓湘凌 | Manufacturing method for gray zirconia ceramics |
| CN108456923A (en) * | 2018-03-27 | 2018-08-28 | 汶川县神州锆业科技有限公司 | Zirconium jewel and its production method |
| CN114059161A (en) * | 2021-06-18 | 2022-02-18 | 汶川县神州锆业科技有限公司 | Zirconium gem composition and method for changing color of zirconium gem composition |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1009285B (en) | 1990-08-22 |
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