CN105036559A - Gem-grade synthesized jadeite pebble and preparation method thereof - Google Patents
Gem-grade synthesized jadeite pebble and preparation method thereof Download PDFInfo
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- CN105036559A CN105036559A CN201510376648.3A CN201510376648A CN105036559A CN 105036559 A CN105036559 A CN 105036559A CN 201510376648 A CN201510376648 A CN 201510376648A CN 105036559 A CN105036559 A CN 105036559A
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Abstract
The invention belongs to the technical field of ceramics, and specifically relates to a semi-transparent gem-grade synthesized jadeite pebble and a preparation method thereof. The preparation method comprises the following steps: weighting 13 to 37 parts by weight of anhydrous sodium carbonate, 38 to 69 parts by weight of pyrophyllite powder, and 0 to 9 parts of amorphous silicon dioxide, fully mixing the weighed raw materials, melting and cooling the mixture to obtain a glass body of jadeite component, grinding the glass body into powder, adding a proper amount of methyl cellulose and water into the glass powder, fully mixing, then granulating, pressing the wet powder into blanks, drying the blanks, sintering the blanks at a high temperature, cooling to obtain glass ceramic sheets; subjecting the glass ceramic sheets to hot isostatic pressure sintering to obtain compact glass ceramic sheets; maintaining the compact glass ceramic sheets under a pressure of 4 to 5 GPa at a temperature of 1250 to 1400 for 0.5 to 1.5 hours, and then slowly cooling to the room temperature and reducing the pressure to the atmospheric pressure so as to obtain the semi-transparent gem-grade synthesized jadeite pebble.
Description
Technical field
The invention belongs to ceramic technology field, be specifically related to a kind of translucent Gem Grade synthesis jadeite seed material and preparation method thereof.
Background technology
Gem Grade synthesis jadeite seed material is actual is a kind of one-component ceramic be made up of jadeite crystalline phase, and pottery is all made up of tiny jadeite crystal, does not substantially have hole (volume density=3.3-3.5g/cm therebetween
3); Gem-jade circle is referred to as synthesis seed material.Jadeite (NaAl [Si
2o
6]) be a kind of chain silicate mineral, oblique system, chain-like structure fundamental mode.The mineral aggregate (can contain other crystalline phase a small amount of) be made up of natural jadeite is commonly called as emerald, is formed in the geologic media of high temperature, high pressure.Therefore, synthesis jadeite is produced under high temperature, high pressure, is called synthetic emerald.Because crystalline phase forms identical, synthesis jadeite has identical chemical composition and crystalline structure with natural jadeite, thus has substantially identical physics and chemistry character.
At present, the common method of synthesizing jadeite seed material is by certain ratio Na with some high-purity industrial raw material and/or chemical reagent
2o:Al
2o
3: SiO
2form admixtion, and by it at 1500 DEG C of high-temperature fusion uniformly glass melt, then the glass sample casting out column is watered by different methods, again column glass sample is cut into certain thickness disk, disk is kept certain hour under 1500 ~ 1700 DEG C of high temperature and 5.6 ~ 6GPa high pressure, after cooling, be synthesis jadeite seed material.
Whether synthesis jadeite seed material is Gem Grade, except its crystalline phase and physical property must reach except the parameters of natural jadeite, mainly sees its transparency and the degree of uniformity of color.Differentiate block sample whether translucent instrument according to be 3 ~ 5 mm thick, two sides is that plane-parallel fast shape sample can through infrared rays, and can provide corresponding to peak; Differentiate sample whether translucent naked eyes vision foundation: the sample of 3 ~ 5 mm thick is under strong-light torch or solar radiation, and entirety presents the scattered light of uniformity.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, object is to provide a kind of translucent Gem Grade synthesis jadeite seed material and preparation method thereof.
For achieving the above object, the technical solution adopted in the present invention is:
A preparation method for translucent Gem Grade synthesis jadeite seed material, is characterized in that, comprise the steps:
(1) raw material is taken by following parts by weight: anhydrous sodium carbonate 13 ~ 37 parts, pyrophyllite in powder 38 ~ 69 parts, 0 ~ 9 part, amorphous silicon di-oxide powder, load weighted raw material is fully mixed, the vitreum of jadeite component is obtained after melting, cooling, the vitreum of jadeite component is ground into glass powder, and this glass powder is the raw material of preparation translucent Gem Grade synthesis jadeite seed material;
(2) add appropriate methylcellulose gum and water, granulation after abundant wet mixing in the glass powder obtained in step (1), wet-milling granulation obtained is pressed into base substrate and dries, then obtains glass-ceramic sheet after high temperature sintering, cooling;
(3) dense glass ceramic plate is obtained after the glass-ceramic sheet that step (2) obtains being carried out HIP sintering;
(4) dense glass ceramic plate is kept 0.5 ~ 1.5 hour under 4 ~ 5GPa, 1250 ~ 1400 DEG C of conditions, then slowly drop to normal temperature and pressure, obtain translucent Gem Grade synthesis jadeite seed material.
In such scheme, the particle diameter of step (1) described glass powder is less than 300 orders.
In such scheme, the add-on of methylcellulose gum described in step (2) is 1 ~ 4wt% of glass powder quality, and the add-on of described water is 8 ~ 15wt% of glass powder quality.
In such scheme, described in step (2), the particle diameter of the wet-milling that granulation obtains is 0.1 ~ 0.3mm.
In such scheme, described in step (2), the pressure of compacting is 15 ~ 20MPa.
In such scheme, the sintering temperature of step (2) described high temperature sintering is 800 ~ 950 DEG C, and sintering time is 1 ~ 3h.
In such scheme, the technique of step (3) described HIP sintering is: 850 ~ 1000 DEG C, sintering 1 ~ 2 hour under 100 ~ 200MPa.
In such scheme, the volume density of the described dense glass ceramic plate of step (3) is 2.55 ± 0.10g/cm
3, the volume density of the described translucent Gem Grade synthesis jadeite seed material of step (3) is 3.4 ± 0.10g/cm
3.
In the present invention, pure translucent Gem Grade synthesis jadeite seed material is white, if want the translucent Gem Grade synthesis jadeite seed material obtaining shades of colour, can add a certain amount of transition ion, as Cr, Mn, Ni, Fe and Ti etc.
The translucent Gem Grade that the preparation method of above-mentioned translucent Gem Grade synthesis jadeite seed material prepares synthesizes jadeite seed material.
Beneficial effect of the present invention is as follows: the translucent Gem Grade synthesis jadeite seed material that preparation method of the present invention prepares is a kind of gem-jade raw material of high-quality, various hardstone jewellery can be processed to and (guard against face to green jade bracelet from emerald, suspension member and hanging piece etc.), there is huge market; The present invention adopts pyrophyllite to be raw material, pyrophyllite is a kind of natural mineral, and the natural multiple element containing trace, can make the composition of synthesis jadeite seed material closer to natural jadeite, color is also closer to natural jadeite, in addition, pyrophyllite enriches in china natural resources, and price is cheap more than other chemical reagent, therefore, preparation method's simple possible of the present invention, cost is low, has great economic worth.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
A kind of translucent Gem Grade synthesis jadeite seed material, prepare by the following method: (1) takes anhydrous sodium carbonate 37 grams, pyrophyllite in powder 69 grams and 9 grams, amorphous silicon di-oxide powder, after load weighted three kinds of raw materials are fully mixed, through obtaining the vitreum of jadeite component after melting, cooling; Then, be ground into by vitreum and be less than 300 object glass powders, this glass powder is the raw material of preparation translucent Gem Grade synthesis jadeite seed material;
(2) in above-mentioned glass powder, add quality is the methylcellulose gum of glass powder quality 1 ~ 4wt% and the water of 8 ~ 15wt%, after abundant wet mixing granulation obtain particle diameter be 0.1 ~ 0.3mm ± wet particulate, the fine granules that will wet is die-filling, adopts friction press at the disc-shaped base substrate of the forming under the pressure of 15 ~ 20MPa to be thickness be 6mm; Dry base substrate, then base substrate is sintered 3 hours at 800 DEG C, with stove cooling, obtaining volume density (D) is 2.24g/cm
3± glass-ceramic sheet;
(3) glass-ceramic sheet is sintered 1 hour under hot isostatic pressing (850 DEG C and 200MPa), obtain D=2.62g/cm
3± dense glass ceramic plate;
(4) dense glass ceramic plate is kept 1.5 hours at 4GPa and 1250 DEG C, after release, obtain white translucent disc-shaped synthesis jadeite seed material.
The volume density of the white translucent synthesis jadeite seed material that the present embodiment prepares is D=3.29g/cm
3±, simultaneously by naked eyes Visual Observations Observations: the sample of 3 ~ 5 mm thick is under strong-light torch or solar radiation, entirety presents the scattered light of uniformity, illustrates that the translucent synthesis jadeite seed material that the present embodiment prepares is Gem Grade translucent synthesis jadeite seed material thus.
Embodiment 2
A kind of translucent Gem Grade synthesis jadeite seed material, prepares: (1) takes anhydrous sodium carbonate 37 grams, pyrophyllite in powder 69 grams and 9 grams, amorphous silicon di-oxide powder and Cr by the following method
2o
30.25 gram, powder, after fully being mixed by load weighted three kinds of raw materials, is placed in crucible and is incubated 2 hours at 1250 DEG C, furnace cooling, obtain the vitreum of jadeite component; Then, be ground into by vitreum and be less than 300 object glass powders, this glass powder is the raw material of preparation translucent Gem Grade synthesis jadeite seed material;
(2) in above-mentioned glass powder, add quality is the methylcellulose gum of glass powder quality 1 ~ 4wt% and the water of 8 ~ 15wt%, after abundant wet mixing granulation obtain particle diameter be 0.1 ~ 0.3mm ± wet particulate, the fine granules that will wet is die-filling, adopts friction press at the disc-shaped base substrate of the forming under the pressure of 15 ~ 20MPa to be thickness be 6mm; Dry base substrate, then base substrate is sintered 1 hour at 850 DEG C, with stove cooling, obtaining volume density (D) is 2.3g/cm
3± glass-ceramic sheet;
(3) glass-ceramic sheet is sintered 2 hours under hot isostatic pressing (1000 DEG C and 100MPa), obtain D=2.61g/cm
3± dense glass ceramic plate;
(4) dense glass ceramic plate is kept 0.5 hour at 5GPa and 1250 DEG C, after release, obtain green semi-transparent circle sheet synthesis jadeite seed material.
The volume density of the green that the present embodiment prepares translucent synthesis jadeite seed material is D=3.31g/cm
3±, simultaneously by naked eyes Visual Observations Observations: the sample of 3 ~ 5 mm thick is under strong-light torch or solar radiation, entirety presents the scattered light of uniformity, illustrates that the translucent synthesis jadeite seed material that the present embodiment prepares is Gem Grade translucent synthesis jadeite seed material thus.
Embodiment 3
A kind of translucent Gem Grade synthesis jadeite seed material, prepare by the following method: (1) takes anhydrous sodium carbonate 13.5 grams, pyrophyllite in powder 38.5 grams, after load weighted two kinds of raw materials are fully mixed, be placed in crucible and be incubated 2 hours at 1250 DEG C, furnace cooling, obtains the vitreum of jadeite component; Then, be ground into by vitreum and be less than 300 object glass powders, this glass powder is the raw material of preparation translucent Gem Grade synthesis jadeite seed material;
(2) in above-mentioned glass powder, add quality is the methylcellulose gum of glass powder quality 1 ~ 4wt% and the water of 8 ~ 15wt%, after abundant wet mixing granulation obtain particle diameter be 0.1 ~ 0.3mm ± wet particulate, the fine granules that will wet is die-filling, adopts friction press at the disc-shaped base substrate of the forming under the pressure of 15 ~ 20MPa to be thickness be 6mm; Dry base substrate, then base substrate is sintered 1 hour at 850 DEG C, with stove cooling, obtaining volume density (D) is 2.34g/cm
3± glass-ceramic sheet;
(3) glass-ceramic sheet is sintered 1.5 hours under hot isostatic pressing (900 DEG C and 150MPa), obtain D=2.6g/cm
3± dense glass ceramic plate;
(4) dense glass ceramic plate is kept 1 hour at 4.5GPa and 1300 DEG C, after release, obtain white translucent disc-shaped synthesis jadeite seed material.
The volume density of the white translucent synthesis jadeite seed material that the present embodiment prepares is D=3.38g/cm
3±, simultaneously by naked eyes Visual Observations Observations: the sample of 3 ~ 5 mm thick is under strong-light torch or solar radiation, entirety presents the scattered light of uniformity, illustrates that the translucent synthesis jadeite seed material that the present embodiment prepares is Gem Grade translucent synthesis jadeite seed material thus.
Embodiment 4
A kind of translucent Gem Grade synthesis jadeite seed material, prepares: (1) takes anhydrous sodium carbonate 13.5 grams, pyrophyllite in powder 38.5 grams and and Cr by the following method
2o
30.25 gram, powder, after fully being mixed by load weighted three kinds of raw materials, is placed in crucible and is incubated 2 hours at 1250 DEG C, furnace cooling, obtain the vitreum of jadeite component; Then, vitreum is ground into-300 object glass powders, this glass powder is the raw material of preparation translucent Gem Grade synthesis jadeite seed material;
(2) in above-mentioned glass powder, add quality is the methylcellulose gum of glass powder quality 1 ~ 4wt% and the water of 8 ~ 15wt%, after abundant wet mixing granulation obtain particle diameter be 0.1 ~ 0.3mm ± wet particulate, the fine granules that will wet is die-filling, adopts friction press at the disc-shaped base substrate of the forming under the pressure of 15 ~ 20MPa to be thickness be 6mm; Dry base substrate, then base substrate is sintered 2 hours at 850 DEG C, with stove cooling, obtaining volume density (D) is 2.32g/cm
3± glass-ceramic sheet;
(3) glass-ceramic sheet is sintered 1 hour under hot isostatic pressing (850 DEG C and 150MPa), obtain D=2.55g/cm
3± dense glass ceramic plate;
(4) dense glass ceramic plate is kept 1.5 hours at 4GPa and 1400 DEG C, after release, obtain green semi-transparent circle sheet synthesis jadeite seed material.
The volume density of the green that the present embodiment prepares translucent synthesis jadeite seed material is D=3.29g/cm
3±, simultaneously by naked eyes Visual Observations Observations: the sample of 3 ~ 5 mm thick is under strong-light torch or solar radiation, entirety presents the scattered light of uniformity, illustrates that the translucent synthesis jadeite seed material that the present embodiment prepares is Gem Grade translucent synthesis jadeite seed material thus.
Obviously, above-described embodiment is only for the example done clearly is described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And therefore amplified apparent change or variation are still within the protection domain of the invention.
Claims (8)
1. a preparation method for translucent Gem Grade synthesis jadeite seed material, is characterized in that, comprise the steps:
(1) raw material is taken by following parts by weight: anhydrous sodium carbonate 13 ~ 37 parts, pyrophyllite in powder 38 ~ 69 parts, 0 ~ 9 part, amorphous silicon di-oxide powder, load weighted raw material is fully mixed, the vitreum of jadeite component is obtained after melting, cooling, the vitreum of jadeite component is ground into glass powder, and this glass powder is the raw material of preparation translucent Gem Grade synthesis jadeite seed material;
(2) add appropriate methylcellulose gum and water, granulation after abundant wet mixing in the glass powder obtained in step (1), wet-milling granulation obtained is pressed into base substrate and dries, then obtains glass-ceramic sheet after high temperature sintering, cooling;
(3) dense glass ceramic plate is obtained after the glass-ceramic sheet that step (2) obtains being carried out HIP sintering;
(4) dense glass ceramic plate is kept 0.5 ~ 1.5 hour under 4 ~ 5GPa, 1250 ~ 1400 DEG C of conditions, then slowly drop to normal temperature and pressure, obtain translucent Gem Grade synthesis jadeite seed material.
2. preparation method according to claim 1, is characterized in that, the particle diameter of step (1) described glass powder is less than 300 orders.
3. preparation method according to claim 1, is characterized in that, the sintering temperature of step (2) described high temperature sintering is 800 ~ 950 DEG C, and sintering time is 1 ~ 3h.
4. preparation method according to claim 1, is characterized in that, the technique of step (3) described HIP sintering is: 850 ~ 1000 DEG C, sintering 1 ~ 2 hour under 100 ~ 200MPa.
5. preparation method according to claim 1, is characterized in that, the add-on of methylcellulose gum described in step (2) is 1 ~ 4wt% of glass powder quality, and the add-on of described water is 8 ~ 15wt% of glass powder quality.
6. preparation method according to claim 1, is characterized in that, described in step (2), the pressure of compacting is 15 ~ 20MPa.
7. preparation method according to claim 1, is characterized in that, described in step (2), the particle diameter of the wet-milling that granulation obtains is 0.1 ~ 0.3mm.
8. the translucent Gem Grade that the arbitrary claim of claim 1 ~ 7 prepares synthesizes jadeite seed material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753466A (en) * | 2016-03-07 | 2016-07-13 | 四川大学 | Synthesis method of polycrystal jade under high pressure |
| CN112592067A (en) * | 2021-01-21 | 2021-04-02 | 新乡学院 | Method for preparing emerald glass ceramics based on phlogopite seed crystals |
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| JPS6086019A (en) * | 1983-10-19 | 1985-05-15 | Seiko Epson Corp | Production of jadeite crystal |
| JPS6096522A (en) * | 1983-10-27 | 1985-05-30 | Seiko Epson Corp | Preparation of jadeite crystal |
| CN1830855A (en) * | 2006-03-09 | 2006-09-13 | 陈志胜 | Artificial emerald jade and its manufacturing method and use |
| CN102060515A (en) * | 2010-11-17 | 2011-05-18 | 昆明理工大学 | Process for preparing synthetic jadeite |
| CN103641313A (en) * | 2013-12-06 | 2014-03-19 | 辽宁红山玉科技有限公司 | Preparation method of bowlder-like microcrystalline glass |
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2015
- 2015-07-01 CN CN201510376648.3A patent/CN105036559B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS6086019A (en) * | 1983-10-19 | 1985-05-15 | Seiko Epson Corp | Production of jadeite crystal |
| JPS6096522A (en) * | 1983-10-27 | 1985-05-30 | Seiko Epson Corp | Preparation of jadeite crystal |
| CN1830855A (en) * | 2006-03-09 | 2006-09-13 | 陈志胜 | Artificial emerald jade and its manufacturing method and use |
| CN102060515A (en) * | 2010-11-17 | 2011-05-18 | 昆明理工大学 | Process for preparing synthetic jadeite |
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| 阎学伟等: "高温高压下翡翠宝石的人工合成", 《高压物理学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753466A (en) * | 2016-03-07 | 2016-07-13 | 四川大学 | Synthesis method of polycrystal jade under high pressure |
| CN112592067A (en) * | 2021-01-21 | 2021-04-02 | 新乡学院 | Method for preparing emerald glass ceramics based on phlogopite seed crystals |
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