CN102060515A - Process for preparing synthetic jadeite - Google Patents
Process for preparing synthetic jadeite Download PDFInfo
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- CN102060515A CN102060515A CN201010547456.1A CN201010547456A CN102060515A CN 102060515 A CN102060515 A CN 102060515A CN 201010547456 A CN201010547456 A CN 201010547456A CN 102060515 A CN102060515 A CN 102060515A
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- Prior art keywords
- jadeite
- ball milling
- emerald
- powder
- temperature
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 229910052640 jadeite Inorganic materials 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000000843 powder Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000007885 magnetic separation Methods 0.000 claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 10
- 241000579895 Chlorostilbon Species 0.000 claims description 46
- 239000010976 emerald Substances 0.000 claims description 46
- 229910052876 emerald Inorganic materials 0.000 claims description 46
- 238000000498 ball milling Methods 0.000 claims description 34
- 238000005516 engineering process Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 239000006148 magnetic separator Substances 0.000 claims description 6
- 239000005308 flint glass Substances 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000005056 compaction Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 4
- 239000011707 mineral Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000000713 high-energy ball milling Methods 0.000 abstract description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 2
- 239000011230 binding agent Substances 0.000 abstract 1
- 235000021190 leftovers Nutrition 0.000 abstract 1
- 230000005389 magnetism Effects 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 235000019580 granularity Nutrition 0.000 description 8
- 239000005331 crown glasses (windows) Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010437 gem Substances 0.000 description 2
- 229910001751 gemstone Inorganic materials 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052892 hornblende Inorganic materials 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Glass Compositions (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides a method for preparing a synthetic jadeite material, which comprises the following steps of: refining leftovers of natural jadeite, performing magnetic separation to remove black or dark-colored materials with magnetism from jadeite powder, adding less than 1 mass percent of Cr2O3 and 1 to 10 mass percent of lead-free colorless glass serving as a binder, proportioning, uniformly mixing in a mixer, and performing low-temperature high-energy ball milling; and prepressing final powder for forming, putting a preformed compact into a discharge plasma reaction synthetic furnace, and sintering at the temperature of between 850 and 1,200 DEG C under the pressure of between 15 and 20KN. By the method, increasingly scarce jadeite mineral resources can be fully utilized, the natural polycrystalline aggregate jadeite is bonded by the discharge plasma sintering process and the like, and the synthetic jadeite material with large volume and high transparency can be prepared on the basis of not changing the crystalline structure of the jadeite.
Description
Technical field
The present invention relates to the stupalith field, particularly relate to the application of artificial preparation gem-jade material and modification aspect.
Background technology
The experiment of synthetic emerald is physics, the electrochemical conditions that the simulation natural jadeite becomes the ore deposit, with the chemical reagent is main raw material, adopt the high temperature solid-state method preparation to have the amorphous glass of emerald composition, utilize the principle of high pressure solid transformation again, on the high-temperature high-pressure apparatus of artificially synthesizing diamond it being carried out thaumatropy handles, make it at emerald stable region intercrystalline, thereby realize the synthetic of artificial emerald.
The raw material that experiment is at present selected for use is chemical pure or analytically pure reagent: Na
2CO
3, Al
2O
3, SiO
2, Cr
2O
3, Li
2CO
3, carry out proportioning with reference to the theoretical composition of natural jadeite basically, be that 0.5%～1.5% ratio of gross weight adds staining agent Cr in Cr constituent content in the natural gemstone level emerald
2O
3After testing, the main crystalline mineral of synthetic emerald is a jadeite, the basically identical of its infrared absorption spectrum and natural jadeite, and the thaumatropy of sample segment is more complete, crystallization degree is better, and conventional gemmary feature such as its hardness, density and specific refractory power and natural jadeite is very close.But because the bad control of crystalline state in the crystalloid process, the color of synthetic emerald and transparency and natural jadeite have very big difference, do not reach the requirement of jewel level.So,, seldom see the goods of synthetic emerald on the market though be that the technology of the synthetic emerald of model reaches its maturity with natural jadeite geology formation condition.
Summary of the invention
The present invention is directed to synthesis technical field for the having relatively high expectations of High Temperature High Pressure, it is synthetic to adopt the natural jadeite powder to carry out secondary.By with quality preferably technologies such as the refinement of natural jadeite scrap stock, magnetic separation, compacting, sintering finally make the emerald goods close with natural jadeite.This invention can make full use of resource in short supply, make that by the low temperature high-energy ball milling causing the look element enters the emerald lattice, by plasma discharging Fast Sintering technology that natural polycrystalline aggregate emerald is bonding again, this technology can be prepared the imitative natural jadeite goods that volume is big, color and luster is controlled on the basis that as far as possible keeps the emerald crystalline structure.Concrete technical matters and method are as follows:
(1) material composition and shared mass percent thereof
Natural jadeite scrap stock, Cr
2O
3Powder (mass percent is less than 1% for purity＞99.9%, granularity 40-50 μ m), unleaded flint glass powder (mass percent is less than 10%), wherein colourless lead-free glass powder mass percent is according to SiO
2(8.45%), Na
2B
4O
7(67.10%) 10H
2O, ZnO (7.98%), Na
2CO
3(5.65%), K
2CO
3(3.89%), NaNO
3(0.32%), Sb
2O
3(9.38%) mix, be heated to 1000 ℃ after behind the furnace cooling grind into powder make.
(2) technical qualification
1. granularity: with natural jadeite scrap stock, crown glass, crushing.Filter out the powdered material of various granularities.Wherein: the emerald powder is 100～200 orders, 80～100 orders, 60～80 orders; Glass powder:＜200 orders.
2. magnetic separation condition: because the relatively poor emerald of quality color and luster often in the scrap stock, dark minerals wherein has the hornblende chromite of electro permanent magnetic more, at first under mineralogical microscope, visible melanocratic mineral is separated, in magnetic separator varigrained emerald powder is carried out the magnetic separation separating treatment then, atrament is separated the back and is obtained transparency emerald powder preferably.
3. mechanical batch mixing: will screen emerald and be bordering on colourless powder and Cr
2O
3Powder and put into planetary temperature control high energy ball mill, abrading-ball and mill jar adopt corundum material preparation, rotating speed 800-1500rad/min, and 5-15 hour ball milling time is (according to Cr
2O
3Content is adjusted), ball milling temperature :-20 ℃-0 ℃.Then leadless glass powder (200 order) is added in the ball grinder rotating speed 500rad/min, 1 hour ball milling time, ball milling temperature :-20 ℃-0 ℃.
4. pressing process takes out the composite granule of preparation from ball grinder, carries out pre-molding by mould, and pressure converts according to the compacting sample rate, need reach half of natural jadeite density.Suppress so that eliminate internal stress by cold isostatic press.
The biscuit compacting pressure
The two-way compacting of punching block: 300-700MPa;
Cold isostatic compaction: 200-400MPa
5. sintering process:
The sample of presuppression is adopted the discharge plasma sintering:
600 ℃-900 ℃ (adjusting according to crown glass content) pressure 20KN of sintering temperature, the employing that heats up heat up stage by stage, and each stage temperature rise rate is greater than 100 ℃/min, and argon shield is incubated 5min, slowly is quickly cooled to room temperature after the release.
(3) compare the advantage that is had with known technology:
1. prepare synthetic emerald with High Temperature High Pressure and compare, that raw material is prepared is simple, technical process is controlled easily, with short production cycle, and can realize producing production process environmentally safe or less contamination in enormous quantities.
2. can effectively improve the raw-material utilization ratio of natural rare emerald,,, all scrap stock can be recycled by present technique because the scrap stock of the emerald course of processing are handled as refuse mostly at present;
3. main body adopts the natural jadeite raw material, can be to greatest extent near the natural jadeite goods, can be prepared into goods such as the suspension member of the various figures of buddha, kwan-yin, hollow out and beading, necklace by processing;
Description of drawings
Fig. 1 is preparation technology's schema of synthetic emerald of the present invention.
Embodiment
Further specify flesh and blood of the present invention below in conjunction with accompanying drawing with example, but content of the present invention is not limited to this.
Embodiment one
With emerald scrap stock, crown glass separated pulverizing, screening.By magnetic separator will be wherein 100～200 orders, 80～100 orders, 60～80 purpose emerald powder carry out the magnetic separation separating treatment, will isolated several granularity emerald powder equal proportions mixing, with Cr
2O
3After powder (mass percent 0.5%), emerald powder (mass percent 98.5%) mix, insert the ball milling that carries out powder in the ball grinder of corundum material.Planetary high-energy ball mill rotating speed 600rad/min, 5 hours ball milling time, ball milling temperature :-20 ℃-0 ℃, 200 order leadless glass powders (mass percent 1%) are inserted rotating speed 500rad/min behind the ball grinder, 0.5 hour ball milling time, ball milling temperature :-20 ℃-0 ℃.The powder of obtaining is inserted mould inside, carries out inserting in the cold isostatic press behind the pre-molding and suppresses.The sample of presuppression is adopted the discharge plasma sintering: 900 ℃ of sintering temperatures; pressure 15KN, temperature rise rate: 30 ℃-400 ℃: 100 ℃/min, 400 ℃-900 ℃: 200 ℃/min, argon shield; insulation 5min, release is taken out sample and is naturally cooled to room temperature.The agglomerating sample is removed the pollution of surface thing, and can to obtain density be 98%, and pale green is sub-translucent reproduces the emerald material.
Embodiment two
With emerald scrap stock, crown glass separated pulverizing, screening.100～200 orders, 80～100 orders, 60～80 purpose emerald powder carry out the magnetic separation separating treatment with inciting somebody to action wherein by magnetic separator, isolated several granularity emerald powder equal proportions are mixed, with Cr
2O
3After powder (mass percent 0.8%) emerald powder (mass percent 94%) mixes, insert the ball milling that carries out powder in the ball grinder of corundum material.High energy ball mill rotating speed 800rad/min, 10 hours ball milling time, ball milling temperature :-20 ℃-0 ℃.200 order leadless glass powders 3% (mass percent) are inserted rotating speed 500rad/min behind the ball grinder, 1 hour ball milling time, ball milling temperature :-20 ℃-0 ℃.The powder of obtaining is inserted mould inside, carries out inserting in the cold isostatic press behind the pre-molding and suppresses.The sample of presuppression is adopted the discharge plasma sintering: 1000 ℃ of sintering temperatures; pressure 18KN, temperature rise rate: 30 ℃-400 ℃: 100 ℃/min, 400 ℃-1200 ℃: 250 ℃/min, argon shield; insulation 5min, release is taken out sample and is naturally cooled to room temperature.The agglomerating sample is removed the pollution of surface thing, and can to obtain density be 98.9%, greenly presses the transparent emerald material that reproduces.
Embodiment three
With emerald scrap stock, crown glass separated pulverizing, screening.100～200 orders, 80～100 orders, 60～80 purpose emerald powder carry out the magnetic separation separating treatment with inciting somebody to action wherein by magnetic separator, isolated several granularity emerald powder equal proportions are mixed, with the Cr of 1% (mass percent)
2O
3After the emerald powder mixes of powder, 98% (mass percent), insert mixing and the refinement of carrying out powder in the ball grinder of corundum material.Planetary high-energy ball mill rotating speed 1000rad/min, 15 hours ball milling time, ball milling temperature :-20 ℃-0 ℃; 200 order leadless glass powders 9% (mass percent) are inserted rotating speed 500rad/min behind the ball grinder, 1.5 hours ball milling time, ball milling temperature :-20 ℃-0 ℃.The powder of obtaining is inserted mould inside, carries out inserting in the cold isostatic press behind the pre-molding and suppresses.The sample of presuppression is adopted the discharge plasma sintering: 1200 ℃ of sintering temperatures; pressure 20KN, temperature rise rate: 30 ℃-400 ℃: 100 ℃/min, 400 ℃-1200 ℃: 300 ℃/min, argon shield; insulation 5min, release is taken out sample and is naturally cooled to room temperature.The agglomerating sample is removed the pollution of surface thing, and can to obtain density be 99.4%, the dark green sub-translucent emerald material that reproduces.
Synthetic emerald preparation methods of the present invention is characterised in that: raw material adopts natural jadeite, causes the look element and adopts Cr
2O
3Black or the dark material that emerald powder inside has magnetic removed in magnetic separation, after preparing burden, in mixer, mix, behind low temperature high energy ball mill ball milling, add unleaded flint glass and carry out ball milling once more, final powder is carried out pre-molding, preformed compact is inserted in the plasma discharging precursor reactant synthetic furnace carry out sintering.
The emerald processing that is chosen as of natural jadeite remains scrap stock or the former stone of inferior quality natural jadeite, and granularity is: 60 orders-200 order.
Cause the look element Cr
2O
3Additive capacity be no more than 1%, by percentage to the quality.
The softening temperature of the unleaded flint glass of additive is no more than 850 ℃, and additive capacity is no more than 10%, by percentage to the quality.
Magnetic separation refers at first by removing the glass powder granularity of interpolation＜200 orders by magnetic separator after the inner dark material of manual removal.
Cause the ball-milling technology that carries out after look element and emerald ball milling mix and to cause the look element relevant, ball milling temperature and ball milling time and to cause the addition of look element relevant, 10-20 hour ball milling time, rotating speed 800-1200rad/min, ball milling temperature :-20 ℃-0 ℃.
Pre-molding base substrate pressure range is: the two-way compacting of punching block: 300-700MPa; Cold isostatic compaction: 200-400MPa.
850 ℃-1200 ℃ of discharge plasma sintering temperatures, pressure 15KN-20KN heats up stage by stage, and each stage temperature rise rate is no more than 100 ℃/min, and insulation 20min cools to room temperature with the furnace after the release.
Claims (8)
1. synthetic emerald preparation methods is characterized in that: raw material adopts natural jadeite, causes the look element and adopts Cr
2O
3Black or the dark material that emerald powder inside has magnetic removed in magnetic separation, after preparing burden, in mixer, mix, behind low temperature high energy ball mill ball milling, add unleaded flint glass and carry out ball milling once more, final powder is carried out pre-molding, preformed compact is inserted in the plasma discharging precursor reactant synthetic furnace carry out sintering.
2. method according to claim 1 is characterized in that, the emerald processing that is chosen as of natural jadeite remains scrap stock or the former stone of inferior quality natural jadeite, and granularity is: 60 orders-200 order.
3. method according to claim 1 is characterized in that, causes the look element Cr
2O
3Additive capacity be no more than 1%, by percentage to the quality.
4. method according to claim 1 is characterized in that: the softening temperature of the unleaded flint glass of additive is no more than 850 ℃, and additive capacity is no more than 10%, by percentage to the quality.
5. method according to claim 1 is characterized in that: magnetic separation refers at first by removing the glass powder granularity of interpolation＜200 orders by magnetic separator after the inner dark material of manual removal.
6. method according to claim 1, it is characterized in that: cause the ball-milling technology that carries out after look element and emerald ball milling mix and cause the look element relevant, the ball milling temperature is relevant with the addition that causes the look element with the ball milling time, 10-20 hour ball milling time, rotating speed 800-1200rad/min, ball milling temperature :-20 ℃-0 ℃.
7. method according to claim 1 is characterized in that: pre-molding base substrate pressure range is: the two-way compacting of punching block: 300-700MPa; Cold isostatic compaction: 200-400MPa.
8. method according to claim 1 is characterized in that: 850 ℃-1200 ℃ of discharge plasma sintering temperatures, and pressure 15KN-20KN heats up stage by stage, and each stage temperature rise rate is no more than 100 ℃/min, and insulation 20min cools to room temperature with the furnace after the release.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010547456.1A CN102060515B (en) | 2010-11-17 | 2010-11-17 | Process for preparing synthetic jadeite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010547456.1A CN102060515B (en) | 2010-11-17 | 2010-11-17 | Process for preparing synthetic jadeite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102060515A true CN102060515A (en) | 2011-05-18 |
| CN102060515B CN102060515B (en) | 2013-03-06 |
Family
ID=43996043
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010547456.1A Expired - Fee Related CN102060515B (en) | 2010-11-17 | 2010-11-17 | Process for preparing synthetic jadeite |
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| Country | Link |
|---|---|
| CN (1) | CN102060515B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961449A (en) * | 2015-07-01 | 2015-10-07 | 中国地质大学（武汉） | Semitransparent jadeite ceramic and preparation method thereof |
| CN105036559A (en) * | 2015-07-01 | 2015-11-11 | 何涌 | Gem-grade synthesized jadeite pebble and preparation method thereof |
| CN105753466A (en) * | 2016-03-07 | 2016-07-13 | 四川大学 | Synthesis method of polycrystal jade under high pressure |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6090813A (en) * | 1983-10-19 | 1985-05-22 | Seiko Epson Corp | Manufacture of jadeite crystal |
| CN1272471A (en) * | 1999-04-29 | 2000-11-08 | 丁民修 | Jadite porcelain and its preparation method |
| CN1343495A (en) * | 2000-09-15 | 2002-04-10 | 金俊汉 | Jadeite extracting agent and its prepn. method |
-
2010
- 2010-11-17 CN CN201010547456.1A patent/CN102060515B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6090813A (en) * | 1983-10-19 | 1985-05-22 | Seiko Epson Corp | Manufacture of jadeite crystal |
| CN1272471A (en) * | 1999-04-29 | 2000-11-08 | 丁民修 | Jadite porcelain and its preparation method |
| CN1343495A (en) * | 2000-09-15 | 2002-04-10 | 金俊汉 | Jadeite extracting agent and its prepn. method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961449A (en) * | 2015-07-01 | 2015-10-07 | 中国地质大学（武汉） | Semitransparent jadeite ceramic and preparation method thereof |
| CN105036559A (en) * | 2015-07-01 | 2015-11-11 | 何涌 | Gem-grade synthesized jadeite pebble and preparation method thereof |
| CN104961449B (en) * | 2015-07-01 | 2017-03-22 | 中国地质大学（武汉） | Semitransparent jadeite ceramic and preparation method thereof |
| CN105753466A (en) * | 2016-03-07 | 2016-07-13 | 四川大学 | Synthesis method of polycrystal jade under high pressure |
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| Publication number | Publication date |
|---|---|
| CN102060515B (en) | 2013-03-06 |
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