CN102060515B - Process for preparing synthetic jadeite - Google Patents

Process for preparing synthetic jadeite Download PDF

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Publication number
CN102060515B
CN102060515B CN201010547456.1A CN201010547456A CN102060515B CN 102060515 B CN102060515 B CN 102060515B CN 201010547456 A CN201010547456 A CN 201010547456A CN 102060515 B CN102060515 B CN 102060515B
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jadeite
ball
temperature
powder
emerald
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CN102060515A (en
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于杰
叶未
陈敬超
冯晶
唐雪莲
杨淼
祖恩东
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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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

A kind of preparation technology of synthetic emerald
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, take chemical reagent as main raw material, adopt the high temperature solid-state method preparation to have the amorphous glass of emerald composition, the principle of recycling high pressure solid transformation, on the high-temperature high-pressure apparatus of artificially synthesizing diamond it being carried out thaumatropy processes, make it at emerald stable region intercrystalline, thereby realize the synthetic of Jadeite.
The raw material that at present experiment is selected is chemical pure or analytically pure reagent: Na 2CO 3, Al 2O 3, SiO 2, Cr 2O 3, Li 2CO 3, basically carry out proportioning with reference to the theoretical composition of natural jadeite, 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 jadeite, its infrared absorption spectrum and natural jadeite basically identical, and the thaumatropy of sample segment is more complete, crystallization degree is better, and the conventional Gemmological Characters such as its hardness, density and specific refractory power and natural jadeite is very close.But because the crystal qualitative Crystallization is controlled out of order, the color of synthetic emerald and transparency and natural jadeite have very large difference, do not reach the requirement of Gem Grade.So, although the technology take natural jadeite geology formation condition as the synthetic emerald of model reaches its maturity, seldom see the goods of synthetic emerald on the market.
Summary of the invention
The present invention is directed to synthesis technical field for the having relatively high expectations of High Temperature High Pressure, adopt the natural jadeite powder to carry out secondary synthetic.By with quality preferably the techniques 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 take full advantage of resource in short supply, enter the emerald lattice by the low temperature high-energy ball milling so that cause the look element, by plasma discharging Fast Sintering technique that natural polycrystalline aggregate emerald is bonding again, this technique can be prepared on the basis that keeps the emerald crystalline structure as far as possible the imitative natural jadeite goods that volume is large, color and luster is controlled.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: jade 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, then in magnetic separator varigrained jade powder is carried out the magnetic separation separating treatment, atrament is separated preferably jade powder of rear acquisition transparency.
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 grinding jar adopt the corundum material preparation, rotating speed 800-1500rad/min, Ball-milling Time 5-15 hour (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, Ball-milling Time 1 hour, 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 in order to 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 with known technology and have advantages of:
1. prepare synthetic emerald with High Temperature High Pressure and compare, that raw material is prepared is simple, technical process is easily controlled, with short production cycle, and can realize producing production process environmentally safe or less contamination in enormous quantities.
2. can the raw-material utilization ratio of the natural rare emerald of Effective Raise, because the scrap stock of the emerald course of processing are processed as refuse mostly at present, by present technique, all scrap stock can be recycled;
3. main body adopts the natural jadeite raw material, can be to greatest extent near the natural jadeite goods, can be prepared into the 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
Emerald scrap stock, crown glass are pulverized respectively screening.By magnetic separator will be wherein 100~200 orders, 80~100 orders, 60~80 purpose jade powders carry out the magnetic separation separating treatment, will isolated several granularity jade powder equal proportions mixing, with Cr 2O 3After powder (mass percent 0.5%), jade 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, Ball-milling Time 5 hours, ball milling temperature :-20 ℃-0 ℃, 200 order leadless glass powders (mass percent 1%) are inserted rotating speed 500rad/min behind the ball grinder, Ball-milling Time 0.5 hour, 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 sample of sintering 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
Emerald scrap stock, crown glass are pulverized respectively screening.100~200 orders, 80~100 orders, 60~80 purpose jade powders carry out the magnetic separation separating treatment with inciting somebody to action wherein by magnetic separator, isolated several granularity jade powder equal proportions are mixed, with Cr 2O 3After powder (mass percent 0.8%) jade 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, Ball-milling Time 10 hours, ball milling temperature :-20 ℃-0 ℃.200 order leadless glass powders 3% (mass percent) are inserted rotating speed 500rad/min behind the ball grinder, Ball-milling Time 1 hour, 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 sample of sintering 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
Emerald scrap stock, crown glass are pulverized respectively screening.100~200 orders, 80~100 orders, 60~80 purpose jade powders carry out the magnetic separation separating treatment with inciting somebody to action wherein by magnetic separator, isolated several granularity jade powder equal proportions are mixed, with the Cr of 1% (mass percent) 2O 3After the jade powder of powder, 98% (mass percent) mixes, 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, Ball-milling Time 15 hours, ball milling temperature :-20 ℃-0 ℃; 200 order leadless glass powders 9% (mass percent) are inserted rotating speed 500rad/min behind the ball grinder, Ball-milling Time 1.5 hours, 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 sample of sintering 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 material preparation method feature of the present invention is: raw material adopts natural jadeite, causes the look element and adopts Cr 2O 3The inner magnetic black of tool of jade powder or dark material are removed in magnetic separation, after batching, in mixer, mix, behind low temperature high energy ball mill ball milling, add unleaded flint glass and carry out again ball milling, 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, Ball-milling Time 10-20 hour, 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 (5)

1. synthetic emerald material preparation method is characterized in that: raw material adopts natural jadeite, causes the look element and adopts Cr 2O 3The inner magnetic black of tool of jade powder or dark material are removed in magnetic separation, after batching, in mixer, mix, behind low temperature high energy ball mill ball milling, add unleaded flint glass and carry out again ball milling, 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;
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;
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, Ball-milling Time 10-20 hour, rotating speed 800-1200rad/min, ball milling temperature :-20 ℃-0 ℃.
2. 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.
3. method according to claim 1, it 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.
4. method according to claim 1 is characterized in that: magnetic separation refers at first to remove the glass powder granularity of interpolation<200 orders by manual by magnetic separator after removing inner dark material.
5. method according to claim 1, it is characterized in that: pre-molding base substrate pressure range is: the two-way compacting of punching block: 300MPa-700MPa; Cold isostatic compaction: 200MPa-400MPa.
CN201010547456.1A 2010-11-17 2010-11-17 Process for preparing synthetic jadeite Expired - Fee Related CN102060515B (en)

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Publication number Priority date Publication date Assignee Title
CN105036559B (en) * 2015-07-01 2017-07-11 何涌 A kind of Gem Grade synthesis jadeite seed material 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

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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Publication number Priority date Publication date Assignee Title
JPS6090813A (en) * 1983-10-19 1985-05-22 Seiko Epson Corp Manufacture of jadeite crystal

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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* Cited by examiner, † Cited by third party
Title
JP昭60-90813A 1985.05.22

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