CN105753466A - Synthesis method of polycrystal jade under high pressure - Google Patents
Synthesis method of polycrystal jade under high pressure Download PDFInfo
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- CN105753466A CN105753466A CN201610125254.5A CN201610125254A CN105753466A CN 105753466 A CN105753466 A CN 105753466A CN 201610125254 A CN201610125254 A CN 201610125254A CN 105753466 A CN105753466 A CN 105753466A
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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Abstract
The invention discloses a synthesis method of polycrystal jade under high pressure. The method comprises: taking anhydrous sodium silicate, alumina and silica powder according to a ratio of n(Na2SiO3):n(Al2O3):n(SiO2)=1:1:3, mixing the substances evenly, then conducting sintering melting at a high temperature of 1200-1800DEG C 2-6 times for 0.5-24h to obtain a compact transparent amorphous jadeite block, and then subjecting the obtained transparent amorphous jadeite block to heat preservation and pressure maintaining under a high pressure of 0.1-15GPa and a high temperature of 1300-2300DEG C for 0.1-48h to crystallize into jadeite ceramic to obtain gem grade jade. The synthesis method provided by the invention has a simple process, and the synthesized sample has a relative density of 3.25-3.38, Mohs hardness of 6.5-7.2, and a refractive index of 1.66 measured by spot measurement technique. After XRD detection, the sample composition is consistent with that of natural jade (PDF card 72-0174), the color is uniform, the texture is mild and humid, and the crystallinity reaches 97-99%, the detection result of a scanning electron microscope to a sample fracture appearance is in accord with that of a natural jade fracture appearance.
Description
Technical field
The invention belongs to jade synthesis field, be specifically related to a kind of method of synthesised polycrystalline jade under high pressure.
Background technology
Emerald, is beautiful one, is the stone matter polycrystalline aggregate reaching beautiful level formed under geologic process, and the chemical composition of the essential mineral of composition emerald is NaAlSi2O6, its mineralogical name is jadeite, and from the point of view of petrology angle, emerald is a kind of rock, the mineral aggregate that it is made up of the Pyroxene Minerals that jadeite is main mineral constituent and amphibole, is a kind of jadeitite or omphacitite, rather than jadeite simple ore object.The essential mineral of composition emerald is percivalite, belong to rhombic prism crystallographic system, it it is typically rhombic prism dress, half rhombic prism dress and irregular particle, there is parallel (001) and the simple twin crystal of (100) and multiple twin, (110) completely cleavage, so by the thicker plaque-like pilotaxitic texture of these mineral compositions and granular mosaic texture, visible cleavage surface and twin plane, namely " the kingfisher property " described in people.Natural jadeite is formed at the polycrystalline jadeite aggregate in high temperature, high pressure geological environment, we by simulation high-temperature and high-pressure conditions can synthesised polycrystalline jadeite in the lab, this polycrystalline jadeite is exactly emerald.
At present, the conventional way of synthesised polycrystalline jade is by a certain proportion of Na2O:Al2O3:SiO2Batch through mixing, the vitreum of jadeite component is obtained after melted, cooling, again the vitreum of jadeite component is ground into glass powder, then by glass powder after machinery pressing mold shaping, by keeping a period of time under 4~5GPa high pressure and 1250~1500 DEG C of high temperature, it is allowed to crystallization and becomes jadeite pottery;Or the raw material after melting waters and builds up column glass sample, then is kept a period of time under 4~5GPa high pressure and 1250~1500 DEG C of high temperature by column glass sample, being allowed to crystallization is jadeite pottery.
In sum, in the title excessively that the vitreum of jadeite component is ground into glass powder, owing to the vitreum hardness of jadeite component is higher, in pulverizing title, no matter it is that hand grinds or magazine is all easily introduced wherein by mechanical crushing, pollute, and the powder pressing mold once again shaping after grinding also causes occurring inside powder pore, the quality making final synthetic emerald will not be fine, it is difficult to obtain the jade emerald of high-quality, therefore, obtain the method for bulky grain high-quality Gem Grade jade by simple technique process and there is certain meaning.
Summary of the invention
Present invention aim at providing a kind of method of synthesised polycrystalline jade under high pressure.
For achieving the above object, the present invention uses technical scheme as follows:
A kind of method of synthesised polycrystalline jade under high pressure, it is characterised in that: its raw material is anhydrous sodium metasilicate, alumina powder, silicon dioxide powder, comprises the steps:
(1) it is n (Na according to the ratio of the amount of material2SiO3): n (Al2O3): n (SiO2)=1:1:3 weighs anhydrous sodium metasilicate, aluminum oxide and silicon dioxide powder respectively, mixes 10~240 minutes;
(2) sintered molten 0.5~24h under the high temperature that the compound obtained in step (1) is placed in 1200~1800 DEG C, sample after melted is cooled to room temperature with the speed of 5~500 DEG C/min, i.e. obtains sub-translucent or translucent amorphous jadeite block;
(3) sintered molten 0.5~24h under the high temperature that the sub-translucent or translucent amorphous jadeite block obtained in step (2) is placed in 1200~1800 DEG C, sample after melted is cooled to room temperature with the speed of 5~1000 DEG C/min, this step 1~5 time repeatedly, finally obtains the transparent amorphous jadeite block of densification;
(4) HTHP sintering: the transparent amorphous jadeite block that will obtain in step (3) heat-insulation pressure keeping 0.1~48h, then decrease temperature and pressure at 0.1~15GPa, 1300~2300 DEG C, obtains translucent jadeite pottery.
In such scheme, in told step (4), increasing temperature and pressure order is: first boost to pressurize behind the 1/4~3/4 of highest pressure, heat up while pressurize, it is incubated after temperature is raised to the 1/4~3/4 of the highest temperature, insulation continues to boost to highest pressure simultaneously, pressurize subsequently is warming up to maximum temperature, then pressure-maintaining and heat-preservation.
In such scheme, described step (1) is added Ca, Cr, Ni, Mn, Mg, the Fe etc. making emerald be shades of colour micro-as coloring agent, such as: make the greeny Cr of emerald3+, the Mn that makes emerald be purple3+, make the Fe that emerald takes on a red color2O3, the 2Fe that makes emerald be yellow2O3·3H2O。
In such scheme, amount is raw material gross mass the 0.01~0.5wt% of described interpolation coloring agent.
Beneficial effects of the present invention is as follows: operation of the present invention is simple, the transparent jadeite block of densification is obtained by high temperature sintering repeatedly, transparent jadeite block after sintering is directly carried out high temperature and pressure experiment, after eliminating abrasive dust die mould there is the drawback of pore in sample interior, and eliminate the step pouring shaping, and the polycrystalline jade utilizing the inventive method to prepare has the various character of Gem Grade jade, various accessories can be processed to, there is huge economic worth.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings, implementation of the present invention is further described
Fig. 1 is at 4.0GPa, the optical photograph of heat-insulation pressure keeping 48h synthetic sample at 1300 DEG C.
Fig. 2 is in 4.0GPa, the XRD spectrum of heat-insulation pressure keeping 48h synthetic sample at 1300 DEG C.
Fig. 3 is at 4.0GPa, the SEM picture of heat-insulation pressure keeping 48h synthetic sample at 1300 DEG C.
Fig. 4 is at 4.5GPa, the optical photograph of heat-insulation pressure keeping 4h synthetic sample at 1400 DEG C.
Fig. 5 is in 4.5GPa, the XRD spectrum of heat-insulation pressure keeping 4h synthetic sample at 1400 DEG C.
Fig. 6 is at 4.5GPa, the SEM picture of heat-insulation pressure keeping 4h synthetic sample at 1400 DEG C.
Fig. 7 is at 5.0GPa, the optical photograph of heat-insulation pressure keeping 10h synthetic sample at 1500 DEG C.
Fig. 8 is in 5.0GPa, the XRD spectrum of heat-insulation pressure keeping 10h synthetic sample at 1500 DEG C.
Fig. 9 is at 5.0GPa, the SEM picture of heat-insulation pressure keeping 10h synthetic sample at 1500 DEG C.
Figure 10 is at 6.0GPa, the optical photograph of heat-insulation pressure keeping 4h synthetic sample at 1600 DEG C.
Figure 11 is in 6.0GPa, the XRD spectrum of heat-insulation pressure keeping 4h synthetic sample at 1600 DEG C.
Figure 12 is at 6.0GPa, the SEM picture of heat-insulation pressure keeping 4h synthetic sample at 1600 DEG C.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A kind of method of synthetic emerald jade under high pressure, is prepared via a method which to obtain: (1) weighs anhydrous sodium metasilicate 3.05g, aluminum oxide 2.50g, silica 4.5g, mixes 60min after adding coloring agent chrome green 0.03g;
(2) mixed raw material is placed under the high temperature of 1200 DEG C and is cooled to room temperature with the speed of 5 DEG C/min after sintered molten 12h, obtain sub-translucent or translucent green amorphous jadeite block;Sub-translucent or the translucent amorphous jadeite block obtained is placed in sintered molten 12h under the high temperature of 1500 DEG C, will melted after sample be cooled to room temperature with the speed of 500 DEG C/min, finally obtain the transparent green amorphous jadeite block of densification;
(3) by the transparent green amorphous jadeite block that obtains in 4.0GPa, heat-insulation pressure keeping 48h, then decrease temperature and pressure at 1300 DEG C, translucent green jadeite crystal is obtained.Concrete increasing temperature and pressure order is: first boost to pressurize after 2GPa, heat up while pressurize, temperature is raised to 700 DEG C of insulations, insulation continues to boost to 4.0GPa simultaneously, pressurize subsequently is warming up to 1300 DEG C, then reducing the temperature to 1100 DEG C of insulations after pressure-maintaining and heat-preservation 48h unload simultaneously and be depressed into 2GPa, pressurize afterwards is cooled to room temperature, finally unloads and is depressed into normal pressure.
The jadeite crystal that the present embodiment prepares is Gem Grade jade, and color mostly is green to emerald green, and sub-translucent-opaque, glassy lustre, relative density is 3.26~3.35, and Mohs' hardness is 6.5-7.1, and it is 1.66 that bayonet point records refractive index.Detecting through XRD, sample composition consistent with natural jadeite (PDF card 72-0174), degree of crystallinity reaches 97%;Surface sweeping Electronic Speculum is basically identical with natural jadeite cross-section morphology to sample section Shape measure result.
Embodiment 2
A kind of method of synthetic emerald jade under high pressure, is prepared via a method which to obtain: (1) weighs anhydrous sodium metasilicate 3.05 grams, 2.50 grams of aluminum oxide, silica 4.5 grams, mixes 60 minutes after adding coloring agent chrome green 0.05 gram;
(2) mixed raw material is placed under the high temperature of 1500 DEG C and is cooled to room temperature with the speed of 30 DEG C/hmin after sintered molten 12h, obtain sub-translucent or translucent green amorphous jadeite block;Sub-translucent or the translucent amorphous jadeite block obtained is placed in melted 4h under the high temperature of 1800 DEG C, will melted after sample be cooled to room temperature with the speed of 1000 DEG C/min, finally obtain the transparent green amorphous jadeite block of densification;
(3) by the transparent green amorphous jadeite block that obtains in 4.5GPa, heat-insulation pressure keeping 4h, then decrease temperature and pressure at 1400 DEG C, translucent green jadeite crystal is obtained.Concrete increasing temperature and pressure order is: first boost to pressurize after 2.5GPa, heat up while pressurize, temperature is raised to 800 DEG C of insulations, insulation continues to boost to 4.5GPa simultaneously, pressurize subsequently is warming up to 1400 DEG C, then reducing the temperature to 1000 DEG C of insulations after pressure-maintaining and heat-preservation 48h unload simultaneously and be depressed into 2GPa, pressurize afterwards is cooled to room temperature, finally unloads and is depressed into normal pressure.
The jadeite crystal that the present embodiment prepares is Gem Grade jade, and color mostly is green to emerald green, and sub-translucent-opaque, glassy lustre, relative density is 3.26~3.31, and Mohs' hardness is 6.5-7.1, and it is 1.66 that bayonet point records refractive index.Detecting through XRD, sample composition consistent with natural jadeite (PDF card 72-0174), degree of crystallinity reaches 98%;Surface sweeping Electronic Speculum reaches consistent to sample section Shape measure result with natural jadeite cross-section morphology.
Embodiment 3
A kind of method of synthetic emerald jade under high pressure, is prepared via a method which to obtain: (1) weighs anhydrous sodium metasilicate 3.05 grams, 2.50 grams of aluminum oxide, silica 4.5 grams, mixes 60 minutes after adding coloring agent chrome green 0.05 gram;
(2) mixed raw material is placed under the high temperature of 1500 DEG C and is cooled to room temperature with the speed of 10 DEG C/min after sintered molten 4h, obtain sub-translucent or translucent green amorphous jadeite block;Sub-translucent or the translucent amorphous jadeite block obtained is placed in sintered molten 4h under the high temperature of 1500 DEG C, will melted after sample be cooled to room temperature with the speed of 100 DEG C/min, finally obtain the transparent green amorphous jadeite block of densification;
(3) by the transparent green amorphous jadeite block that obtains in 5.0GPa, heat-insulation pressure keeping 10h, then decrease temperature and pressure at 1500 DEG C, translucent green jadeite crystal is obtained.Concrete increasing temperature and pressure order is: first boost to pressurize after 2.5GPa, heat up while pressurize, temperature is raised to 800 DEG C of insulations, insulation continues to boost to 5.0GPa simultaneously, pressurize subsequently is warming up to 1500 DEG C, then reducing the temperature to 1000 DEG C of insulations after pressure-maintaining and heat-preservation 48h unload simultaneously and be depressed into 2GPa, pressurize afterwards is cooled to room temperature, finally unloads and is depressed into normal pressure.
The jadeite crystal that the present embodiment prepares is Gem Grade jade, and color mostly is green to emerald green, and sub-translucent-opaque, glassy lustre, relative density is 3.26~3.32, and Mohs' hardness is 6.5-7.1, and it is 1.66 that bayonet point records refractive index.Detecting through XRD, sample composition consistent with natural jadeite (PDF card 72-0174), degree of crystallinity reaches 98%;Surface sweeping Electronic Speculum reaches consistent to sample section Shape measure result with natural jadeite cross-section morphology.
Embodiment 4
A kind of method of synthetic emerald jade under high pressure, is prepared via a method which to obtain: (1) weighs anhydrous sodium metasilicate 3.05 grams, 2.50 grams of aluminum oxide, silica 4.5 grams, mixes 60 minutes after adding coloring agent chrome green 0.05 gram;
(2) mixed raw material is placed under the high temperature of 1500 DEG C and is cooled to room temperature with the speed of 50 DEG C/min after sintered molten 8h, obtain sub-translucent or translucent green amorphous jadeite block;Sub-translucent or the translucent amorphous jadeite block obtained is placed in sintered molten 10h under the high temperature of 1600 DEG C, will melted after sample be cooled to room temperature with the speed of 500 DEG C/min, finally obtain the transparent green amorphous jadeite block of densification;
(3) by the transparent green amorphous jadeite block that obtains in 6.0GPa, heat-insulation pressure keeping 4h, then decrease temperature and pressure at 1600 DEG C, translucent green jadeite crystal is obtained.Concrete increasing temperature and pressure order is: first boost to pressurize after 3GPa, heat up while pressurize, temperature is raised to 1000 DEG C of insulations, insulation continues to boost to 6.0GPa simultaneously, pressurize subsequently is warming up to 1600 DEG C, then reducing the temperature to 1100 DEG C of insulations after pressure-maintaining and heat-preservation 48h unload simultaneously and be depressed into 3GPa, pressurize afterwards is cooled to room temperature, finally unloads and is depressed into normal pressure.
The jadeite crystal that the present embodiment prepares is Gem Grade jade, and color mostly is green to emerald green, and sub-translucent-opaque, glassy lustre, relative density is 3.26~3.35, and Mohs' hardness is 6.7-7.2, and it is 1.66 that bayonet point records refractive index.Detecting through XRD, sample composition consistent with natural jadeite (PDF card 72-0174), degree of crystallinity reaches 99%;Surface sweeping Electronic Speculum reaches consistent to sample section Shape measure result with natural jadeite cross-section morphology.
Claims (4)
1. the method for synthesised polycrystalline jade under a high pressure, it is characterised in that: its raw material is anhydrous sodium metasilicate, alumina powder, silicon dioxide powder, comprises the steps:
It is n (Na according to the ratio of the amount of material2SiO3): n (Al2O3): n (SiO2)=1:1:3 weighs anhydrous sodium metasilicate, aluminum oxide and silicon dioxide powder respectively, mixes 10~240 minutes;
The compound obtained in step (1) is placed in sintered molten 0.5~24h under the high temperature of 1200~1800 DEG C, the sample after melted is cooled to room temperature with the speed of 0.5~1000 DEG C/min, i.e. obtains sub-translucent or translucent amorphous jadeite block;
Sintered molten 0.5~24h under the high temperature that the sub-translucent or translucent amorphous jadeite block obtained in step (2) is placed in 1200~1800 DEG C, sample after melted is cooled to room temperature with the speed of 0.5~1000 DEG C/min, this step 1~5 time repeatedly, finally obtains the transparent amorphous jadeite block of densification;
HTHP sinters: transparent amorphous jadeite block heat-insulation pressure keeping 0.1~48h, the then decrease temperature and pressure at 0.1~15GPa, 1300~2300 DEG C that will obtain in step (3), obtains translucent jadeite pottery.
The method of synthesised polycrystalline jade under high pressure the most according to claim 1, it is characterised in that: the ratio of the amount of described raw material material is n (Na2SiO3): n (Al2O3·SiO2The sodium metasilicate of)=1:1 substitutes with aluminium silicate powder, or is n (NaOH): n (Al with the ratio of the amount of material2O3): n (SiO2The NaOH of)=2:1:4, aluminum oxide substitute with silicon dioxide powder;Or it is n (Na with the ratio of the amount of material2CO3): n (Al2O3): n (SiO2The sodium carbonate of)=1:1:4, aluminum oxide substitute with silicon dioxide powder.
3. according to the method for synthesised polycrystalline jade under the arbitrary described high pressure of claim 1 or 2, it is characterised in that: in described step (1), add Ca, Cr, Ni, Mn, Mg, the Fe etc. making emerald be shades of colour micro-as coloring agent.
The method of synthesised polycrystalline jade under high pressure the most according to claim 3, it is characterised in that: amount is raw material gross mass the 0.01~0.5wt% of described interpolation coloring agent.
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Cited By (5)
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CN110683763A (en) * | 2019-11-28 | 2020-01-14 | 新乡学院 | Emerald vitreous glaze and glazing method |
CN112592066A (en) * | 2021-01-21 | 2021-04-02 | 新乡学院 | Method for preparing emerald microcrystalline glass |
CN113291086A (en) * | 2021-05-12 | 2021-08-24 | 洛阳职业技术学院 | Development and production method of tourist souvenir |
CN115321569A (en) * | 2022-07-25 | 2022-11-11 | 四川大学 | Preparation method of diaspore |
CN117904714A (en) * | 2024-01-22 | 2024-04-19 | 深圳市东方聚成科技有限公司 | Method for synthesizing polycrystalline jadeite |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110683763A (en) * | 2019-11-28 | 2020-01-14 | 新乡学院 | Emerald vitreous glaze and glazing method |
CN112592066A (en) * | 2021-01-21 | 2021-04-02 | 新乡学院 | Method for preparing emerald microcrystalline glass |
CN113291086A (en) * | 2021-05-12 | 2021-08-24 | 洛阳职业技术学院 | Development and production method of tourist souvenir |
CN115321569A (en) * | 2022-07-25 | 2022-11-11 | 四川大学 | Preparation method of diaspore |
CN115321569B (en) * | 2022-07-25 | 2024-05-10 | 四川大学 | Preparation method of diaspore |
CN117904714A (en) * | 2024-01-22 | 2024-04-19 | 深圳市东方聚成科技有限公司 | Method for synthesizing polycrystalline jadeite |
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