CN1195717A - Method and device for growing diamond of aureoviridae family - Google Patents
Method and device for growing diamond of aureoviridae family Download PDFInfo
- Publication number
- CN1195717A CN1195717A CN97106365A CN97106365A CN1195717A CN 1195717 A CN1195717 A CN 1195717A CN 97106365 A CN97106365 A CN 97106365A CN 97106365 A CN97106365 A CN 97106365A CN 1195717 A CN1195717 A CN 1195717A
- Authority
- CN
- China
- Prior art keywords
- crucible
- chrysoberyl
- melt
- crystal
- growth
- Prior art date
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000010432 diamond Substances 0.000 title abstract 2
- 229910003460 diamond Inorganic materials 0.000 title abstract 2
- 239000013078 crystal Substances 0.000 claims abstract description 38
- 239000010437 gem Substances 0.000 claims abstract description 23
- 229910001751 gemstone Inorganic materials 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000000155 melt Substances 0.000 claims abstract description 7
- 229910001602 chrysoberyl Inorganic materials 0.000 claims description 39
- 239000002994 raw material Substances 0.000 claims description 24
- 241000282326 Felis catus Species 0.000 claims description 14
- NNBFNNNWANBMTI-UHFFFAOYSA-M brilliant green Chemical compound OS([O-])(=O)=O.C1=CC(N(CC)CC)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](CC)CC)C=C1 NNBFNNNWANBMTI-UHFFFAOYSA-M 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000007246 mechanism Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000005441 aurora Substances 0.000 abstract 3
- 241000579895 Chlorostilbon Species 0.000 abstract 1
- 239000010976 emerald Substances 0.000 abstract 1
- 229910052876 emerald Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007716 flux method Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- NHDHVHZZCFYRSB-UHFFFAOYSA-N pyriproxyfen Chemical compound C=1C=CC=NC=1OC(C)COC(C=C1)=CC=C1OC1=CC=CC=C1 NHDHVHZZCFYRSB-UHFFFAOYSA-N 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A method and device for growing a diamond of the family of emerald gems. The family of aurora includes aurora, aurora and alexandrite. These three gemstones are mainly used for ornamental purposes. The growth method of the invention is a rotary temperature gradient method, and the growth device is a rotary temperature gradient furnace. The method is characterized in that the crystal growth process is from the bottom of the melt to the top, the crucible can rotate or move up and down, the rotation of the crucible can fully mix the melt in the melt, the required impurities are supplemented or supplemented from the top of the crucible, and the grown gem crystal is high-quality. The equipment is relatively simple, and the ratio of output to input is high.
Description
The present invention relates to a kind of method and device thereof of the chrysoberyl family non-functional jewel of growing.The crystal of chrysoberyl family comprises the purple emerald green alexandrite (Alexandrite) of chrysoberyl cat's eye (Chrysoberyl Cat ' s Eye), chrysoberyl (English name Chrysoberyl) and Alexandria, mainly is applicable to the ornaments industry.
Prior art: the above-mentioned jewel that people like, natural resource seldom cost an arm and a leg, thus nineteen forties just the someone attempt in all sorts of ways and carry out synthetic growth.The method that adopts has scorification (melting), liquation method (molten solution technique), hydrothermal method (hydrothermal), flame method (verneuil method) and flux method (flux method).But the former crystalline substance of the jewel that these methods obtain is very little, the meaning of not growing.Particular case can be consulted G.A.Bukin et al, " Growth of Alexandrite Crystals and Investigation of their Properties ", Journal of Crystal Growth, 52 (1981), 537～541.North-Holland PublishingCompany, 537 pages at the 1st joint; 539 pages at the 3rd joint; With E.F.Farrell et al, " Flux Growth ofChrysoberyl and Alexandrite ", J.Amer.Ceramic Soc., 47 (1964) 274～276. later 1970s, begin with the purple emerald green alexandrite of crystal pulling method (Czochralski Method) growth Alexandria and obtained high-tech application; See J.C.Walling et al, " Tunable Alexandrite Lasers " IEEE Journal ofQuantum Electronics, QE16 (12), the (1980) 1302～1315, the 2nd joint, 1304 pages.But because of cost high not as the ornaments jewel.1994, Chinese Academy of Sciences's Shanghai ray machine began to provide civilian Alexandria purple emerald green alexandrite non-functional jewel, sees Shen Guorong chief editor " Chinese practical scientific and technological achievement voluminous dictionary ", press of Southwest Jiaotong University, version in 1994,617 pages, the 12020901st " laser crystals and jewel "; With also be Czochralski grown.
Crystal pulling method is raw material to be put into iridium crucible be fused into melt, allows seed crystal contact bath surface under proper temperature, the lifting crystal growth that slowly makes progress then.Crystal diameter is limited to 1/3～1/2 of crucible bore, and, have only 1/4 raw material can be drawn as color and luster available crystal.Crystal pulling method equipment complexity in addition, the technical requirements harshness, so be used for producing the purple emerald green alexandrite of civilian Alexandria, output/output-input ratio is low, is unfavorable for producing in batches.This is a weak point of existing crystal pulling method.In addition, crystal pulling method is difficult to produce chrysoberyl cat's eye, and this is because the valence state of adulterated titanium ion can not get optimum control.So also nobody produces chrysoberyl cat's eye and chrysoberyl so far.
(Rotational thermal gradient method RTG) and use the rotation gradient furnace purple emerald green alexandrite of civilian chrysoberyl cat's eye, chrysoberyl and Alexandria of growing, reaches the purpose of batch process to the objective of the invention is to adopt the warm terraced method of rotation.Mainly be the synthetic technology that solves chrysoberyl cat's eye, also solve the batch process problem of civilian chrysoberyl and purple emerald green alexandrite simultaneously, overcome a shortcoming and a difficult problem in the prior art.
The used device of the present invention be through the terraced method single crystal growing furnace of improved temperature be have the rotation travel mechanism 14, be called the rotation gradient furnace.Fig. 1 is the internal structure of rotation gradient furnace body of heater.Wherein used crucible 1 can be processed into by the molybdenum ingot, and its diameter is equivalent to the diameter of the former crystalline substance of wanting, and its height is greater than the length of former crystalline substance.The inner cylinder of crucible 1 has 1: 100 gradient, is beneficial to pouring out of former crystalline substance; There is The Small Well 2 crucible 1 bottom to place seed crystal.In addition, be furnished with crucible cover 3, according to different jewels, the crucible cover 3 that varies in size with atresia or perforate is with the influence of control furnace atmosphere to crystal growth.Hold raw material melt 4 in the crucible 1.Crucible 1 is placed on the crucible tray 5 that is supported by crucible pole 6, and crucible pole 6 has rotation travel mechanism 14, and rotation travel mechanism 14 can make crucible tray 5 ask crucible 1 to rotate together or move up and down.Velocity of rotation R=0～100 rev/min.Crucible 1 is to place in the heating element 7, and heating element 7 can be processed by high purity graphite, and the cylinder of the rectangular wavy power circuit of its shape is seen Fig. 2.Power by the electrode on the external power 13 with 8 pairs of heating elements of Graphite Electrodes clamping plate 7 that heating element 7 links.The support ring 9 that alundum tube is made is supporting electrode clamping plate 8.Temperature-control heat couple 10 and temperature thermocouple 11 are the W-Re thermocouple, extend near the heating element 7 respectively and near crucible 1 bottom.In order to reach necessary high temperature, heating element 7 up and down and heat protection screen 12 is all arranged on every side, heat protection screen 12 can be made with molybdenum sheet.
The detailed process of growing crystal is as follows:
Three kinds of basic dynamic processes of jewel synthetic are similar.Their basic raw material also is identical, i.e. Al
2O
3And BeO, the impurity difference of just mixing.At first be to choose highly purified raw material, Al
2O
3With BeO and the impurity raw material mixed.The importantly processing of BeO raw material.The present invention is individual curing BeO (comprising briquetting and weighing) in airtight operation box system, not with Al
2O
3Mix (promptly not batch mixing), guarantee to dwindle protective range.Al
2O
3Only mix the back briquetting mutually with adulterated impurity.Material purity is 99.99%.Composition of raw materials is calculated as follows respectively:
(1) chrysoberyl cat's eye:
(1-x-y)Al
2O
3+xFe
2O
3+2yTiO
2+BeO＝BeAl
2-2x-2yFe
2xTi
2yO
4+...
(2) chrysoberyl:
(1-x)Al
2O
3+xFe
2O
3+BeO＝BeAl
2-2xFe
2xO
4
(3) the purple emerald green alexandrite of Alexandria:
(1-t-u) Al
2O
3+ tCr
2O
3+ uV
2O
5+ BeO=BeAl
2-2t-2uCr
2tV
2uO
4+ uO
2X=0～0.1 wherein, y=0～0.2, t=0～0.01, u=0～0.01.Load weighted TiO
2Preferably after handling, reduction becomes Ti
2O
3Use again.
At first in the The Small Well 2 of crucible 1 afterbody, put into seed crystal, also can not put.With the raw material block crucible 1 of packing into of preparation, cover crucible cover 3 then.To vacuumize in the stove, when vacuum tightness reaches 10
-5Charge into the high-purity argon gas of certain pressure behind the torr.Slowly be warming up to 1900 ℃ and allow raw material melt, the rotating speeds rotation crucible 1 with about 10～20 rev/mins allows melt mix.At last, the crystal of follow procedure cooling growth.Temperature control is realized by YC series Program for precision temperature controller.
Key of the present invention is from melt bottom beginning growing crystal.This successful growth to the chrysoberyl group crystal of raw material ratio heavy phase difference great disparity is very favourable.In addition, often spontaneous reducing atmosphere carbon monoxide in this stove is of value to trivalent Ti impurity and enters lattice, synthetic chatoyant.
Method of the present invention is the warm terraced method of rotation, rotating speed R=0～100 rev/min; When R=0, promptly be warm terraced method.When growing above-mentioned crystal, promptly be called descent method when crucible pole 6 drive crucibles, 1 decline.Also having heat-exchanging method also is from melt bottom beginning growing crystal.Be the color that satisfies jewel and the requirement of tone, adulterated impurity comprises V, Cr, Mn, Fe, Co, Ni, Ti, and doping content is in 0～50at% scope.In order to improve output and color even, by crucible 1 top continuous charging with add assortedly, also belong to one of characteristics that the present invention can accomplish.The crystalline aftertreatment, promptly annealing process is important for jewel.The crystal that grows up to is cut into sheet and anneals after taking out; Annealing temperature T 〉=1000 ℃, hold-time t 〉=24 hour; Annealing is to carry out in air or the while aerating oxygen.Institute of the present invention growing crystal annealed aftertreatment also has one's own knack, and more is absolutely necessary when producing chrysoberyl cat's eye and chrysoberyl.
Advantage of the present invention: rotation gradient furnace that the present invention adopts and the warm terraced method of rotation are the best method of producing the above-mentioned three kinds of civilian non-functional jewels that belong to chrysoberyl mineral family.Because of crystal growing process is from the melt bottom, crucible rotates can make the different raw material melt thorough mixing of proportion again, has improved yield rate; Can from the perforate of crucible cover 3, add impurity or raw material continuously, help the scale production of the above-mentioned jewel of fine.With this advantage, filled up the industry blank.Equipment is simple relatively, output/output-input ratio height.Furnace atmosphere can obtain suitable control to the influence of crystal growth.Especially chrysoberyl cat's eye helps the lattice that enters of Ti with method of the present invention, forms chatoyance.Three kinds of jewels of the purple emerald green alexandrite of chrysoberyl cat's eye, chrysoberyl and Alexandria all are rare special jewels, cost an arm and a leg; Have a large capacity and a wide range in the commercial market.
Description of drawings:
Fig. 1 is the structural representation of the used rotation gradient furnace of the present invention
Fig. 2 is the shape synoptic diagram of heating element 7
Embodiment 1: the growth of chrysoberyl cat's eye
Select raw material A l
2O
3With the purity of BeO be 99.99%, adulterated Fe
2O
3And TiO
2Purity is 99.9%.At first with TiO
2In hydrogen, do high temperature reduction and handle, generate Ti
2O
3Standby.Prescription is calculated as follows:
(1-x-y) Al
2O
3+ xFe
2O
3+ 2yTiO
2+ BeO=Fe: Ti: BeAl
2O
4X=0.005 wherein, y=0.04～0.08;
With load weighted Al
2O
3, Fe
2O
3, and the TiO that handles through reduction
2, mix briquetting.Then briquetting, weighing separately in the seal operation case of BeO.Utilize the molybdenum crucible 1 of Φ 80 * 180mm.Earlier with c-axle BeAl
2O
4Seed crystal is put into the The Small Well 2 at the bottom of the crucible, also can not put.Press Al then
2O
3---BeO---Al
2O
3---BeO---Al
2O
3Alternately add, add whole last Al at last
2O
3, with the raw material block crucible 1 of packing into.Cover crucible cover 3 with two Φ 10mm through holes.Be evacuated to 10 in the burner hearth
-5Torr charges into pure argon.Automatically be warmed up to 1900 ℃ of temperature thermocouple indications, raw material becomes melt in the crucible 1, and rotating crucible, is changeed and stopped one minute in two minutes, six times repeatedly by rotating speed R=16 rev/min.Then, follow procedure cooling growing crystal, 2.5 ℃/hour of rate of temperature fall.In the process of growth, crucible rotation R=28 rev/min (also can not changeing).Through 16 hours stove is reduced to room temperature again.
The crystal that takes out is cut into the thick slice, thin piece of 1.2cm, puts into muffle furnace, carries out in the air (but also aerating oxygen) annealing.Annealing temperature T=1200～1300 ℃, annealing time t=24 hour.
Embodiment 2: the growth of chrysoberyl
Choose raw material A l
2O
3With the purity of BeO be 99.99%, the content that contains Ca, Mg, Na, Si impurity all must not surpass 80ppm, 100ppm, 100ppm, 80ppm respectively.Fe
2O
3Purity be 99.9%.Prescription is calculated as follows:
(1-x) Al
2O
3+ xFe
2O
3+ BeO=Fe: BeAl
2O
4Wherein, x=0.005～0.01.With load weighted Al
2O
3And Fe
2O
3Mix briquetting, the independent briquetting of BeO, weighing.Crucible, seed crystal and put packing into of method, raw material block are all with embodiment 1.Cover the crucible cover 3 of atresia.The following steps such as inflation of finding time to annealing process also with embodiment 1.
Embodiment 3: the growth of the purple emerald green alexandrite of Alexandria
Choose raw material A l
2O
3With the purity of BeO be 99.99%, contain impurity Ca, Mg, Na, Si are no more than 100ppm respectively.Cr
2O
3Purity be 99.9%.Prescription is calculated as follows:
(1-t-u) Al
2O
3+ tCr
2O
3+ uV
2O
5+ BeO=Cr: V: BeAl
2O
4+ ... wherein, t=0.0012～0.0016, u=0～0.0018.
Following technology such as raw material weighing is entirely with embodiment 2, but the crystal that obtains need not be annealed.
Claims (5)
1. the growth method of a chrysoberyl family non-functional jewel.Chrysoberyl family comprises chrysoberyl cat's eye, chrysoberyl and the purple emerald green alexandrite of Alexandria, it is characterized in that beginning the process of growing crystal upwards from the melt bottom, and melt is to rotate to move, and is called the warm terraced method of rotation.
2. the growing apparatus of a chrysoberyl family non-functional jewel, its body of heater comprises and placing in the heating element (7), on the crucible tray (5) that supports by crucible pole (6), the crucible (1) that holds raw material melt (4) and be stamped crucible cover (3) is arranged, the The Small Well (2) of putting seed crystal is arranged at the bottom of crucible (1), heating element (7) has the electrode clamping plate (8) and the electrode (13) that are supported by support ring (9) to link with external power, heating element (7) up and down around heat protection screen (12) all arranged, press close to heating element (7) and crucible (1) bottom temperature-control heat couple (10) and temperature thermocouple (11) are arranged, the crucible pole (6) that it is characterized in that support crucible holder (5) and crucible (1) has rotation travel mechanism (14), can drive crucible (1) and rotate together and move, so claim to rotate gradient furnace.
3. according to the growth method of the chrysoberyl family non-functional jewel of claim 1, the concrete composition of raw materials of the purple emerald green alexandrite of chrysoberyl cat's eye, chrysoberyl and Alexandria that it is characterized in that growing is:
[1] chrysoberyl cat's eye is:
(1-x-y)Al
2O
3+xFe
2O
3+2yTiO
2+BeO＝BeAl
2-2x-2yFe
2xTi
2yO
4+…
[2] chrysoberyl is:
(1-x)Al
2O
3+xFe
2O
3+BeO＝BeAl
2-2xFe
2xO
4
[3] the purple emerald green alexandrite of Alexandria is:
(1-t-u)Al
2O
3+tCr
2O
3+uV
2O
5+BeO＝BeAl
2-2t-2uCr
2tV
2uO
4+uO
2
In the following formula, x=0～0.1, y=0～0.2, t=0～0.01, u=0～0.01.
4. according to the growing apparatus of the chrysoberyl family non-functional jewel of claim 2, it is characterized in that rotating speed of rotation R=0～100 rev/min of gradient furnace.
5. according to the growth method of the chrysoberyl family non-functional jewel of claim 1 or 3, it is characterized in that idiographic flow mainly is:
[1] chooses high-purity raw Al
2O
3With adulterated impurity weighing, mix, briquetting;
[2] choose high-purity raw BeO, briquetting, weighing separately in airtight operation box;
[3] raw material of preparation is put into crucible (1);
[4] be evacuated to vacuum tightness in the stove and reach 10
-5During torr, charge into argon gas;
[5] intensification makes the raw material fusing form melt (4) in the stove; Rotation crucible (1) mixes the melt in the melt (4), in the process of growth, and the speed of rotation R of crucible (1), perhaps R＞0, perhaps R=0;
[6] follow procedure is to the crystal cooling of growth, and temperature is reduced to room temperature, and growth ending takes out crystal;
[7] chrysoberyl cat's eye, chrysoberyl are carried out anneal, annealing temperature T＞1000 ℃, anneal in air in annealing time t 〉=24 hour, or aerating oxygen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106365A CN1062318C (en) | 1997-04-08 | 1997-04-08 | Method and device for growing diamond of aureoviridae family |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106365A CN1062318C (en) | 1997-04-08 | 1997-04-08 | Method and device for growing diamond of aureoviridae family |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1195717A true CN1195717A (en) | 1998-10-14 |
| CN1062318C CN1062318C (en) | 2001-02-21 |
Family
ID=5168612
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97106365A Expired - Fee Related CN1062318C (en) | 1997-04-08 | 1997-04-08 | Method and device for growing diamond of aureoviridae family |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1062318C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104073872A (en) * | 2014-06-26 | 2014-10-01 | 大庆佳昌晶能信息材料有限公司 | Process for growing high-quality compound semiconductor single crystal by means of rotation-vertical gradient freeze (R-VGF) method |
| CN104197711A (en) * | 2014-09-19 | 2014-12-10 | 重庆科技学院 | Rotating half occluded thermal shock sintering resistance furnace |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5438299A (en) * | 1977-08-31 | 1979-03-22 | Kyoto Ceramic | Alexandrite sythetic single crystal |
-
1997
- 1997-04-08 CN CN97106365A patent/CN1062318C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104073872A (en) * | 2014-06-26 | 2014-10-01 | 大庆佳昌晶能信息材料有限公司 | Process for growing high-quality compound semiconductor single crystal by means of rotation-vertical gradient freeze (R-VGF) method |
| CN104197711A (en) * | 2014-09-19 | 2014-12-10 | 重庆科技学院 | Rotating half occluded thermal shock sintering resistance furnace |
| CN104197711B (en) * | 2014-09-19 | 2015-12-23 | 重庆科技学院 | One is rotary partly blocks thermal shock sintering resistance furnace |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1062318C (en) | 2001-02-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CZ303673B6 (en) | Preparation of doped garnet structure single crystals with diameters of up to 500 mm | |
| CN102168307B (en) | Method for growing cerium-yttrium-aluminum garnet crystal | |
| CN101580961A (en) | Method for growing crystal by reducing atmosphere Kyropoulos method | |
| CN102758249A (en) | Method for preparing colorless corundum monocrystal | |
| CN101054723A (en) | Method for growing R-surface sapphire crystal | |
| CN1225572C (en) | Integrated melt method for crystal growth | |
| CN114164485A (en) | Method for doping FeSe superconductor material with Si and Te elements together | |
| CN110318097B (en) | Preparation method of lanthanum gallium niobate single crystal | |
| LU503019B1 (en) | Method for preparing single-crystal pyrope under high-temperature and high-pressure condition | |
| CN1195717A (en) | Method and device for growing diamond of aureoviridae family | |
| McEwen et al. | Crystal growth of the rare earth metals | |
| Ginley et al. | Preparation and czochralski crystal growth of the iron titanates, FeTiO3, Fe2TiO4, and Fe2TiO5 | |
| WO2012060050A1 (en) | Quartz glass crucible, method for producing same, and method for producing monocrystalline silicon | |
| Baughman | Preparation and single crystal growth of PtGa2 and AuX2 compounds | |
| Lomonova et al. | Growth of zirconia crystals by skull‐melting technique | |
| LU503141B1 (en) | Method for preparing high-nickel, high-zinc and high-water single-crystal diopside under high-temperature and high-pressure condition | |
| CN101407402B (en) | Preparation method of beryllium aluminate crystal substrate color changing gem | |
| Garton et al. | Crystal growth of some rare earth trifluorides | |
| CN101054725A (en) | Method for growing lithium aluminate crystal | |
| LU503139B1 (en) | Method for preparing single-crystal spessartine under high-temperature and high-pressure condition | |
| LU503140B1 (en) | Method for preparing high-titanium, high-vanadium, high-chromium and high-water single-crystal monticellite | |
| JPS58104100A (en) | Growth process for smco5 single crystal | |
| CN113862786B (en) | Terbium vanadium niobate yttrium magneto-optical crystal and preparation method thereof | |
| CN118600549A (en) | Synthesis system and method of gallium antimonide polycrystal | |
| CN117626432A (en) | Method for eliminating 1.7-2.0 mu m absorption peak of disordered gallium lanthanum silicate crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |