CN106544730A - A kind of ruby preparation method of synthetic major diameter - Google Patents
A kind of ruby preparation method of synthetic major diameter Download PDFInfo
- Publication number
- CN106544730A CN106544730A CN201710053444.5A CN201710053444A CN106544730A CN 106544730 A CN106544730 A CN 106544730A CN 201710053444 A CN201710053444 A CN 201710053444A CN 106544730 A CN106544730 A CN 106544730A
- Authority
- CN
- China
- Prior art keywords
- crystal
- blanking
- ruby
- preparation
- major diameter
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Glass Compositions (AREA)
Abstract
The invention belongs to the preparation method technical field of artificial intraocular lensess, the ruby preparation method of more particularly to a kind of synthetic major diameter.Technical problem solved by the invention is to provide a kind of evenness, improves effective rate of utilization, reduces the ruby preparation method of synthetic major diameter of production cost, comprises the steps：A, addition raw material：B, slotting crystal seed；C, igniting：Light oxyhydrogen；D, sintering crystal；Wherein, step D sintering crystal includes procedure below：(1) material crystallization；(2) to center；(3) crystal expands；(4) isodiametric growth.E, blowing out cooling obtain final product crystal.Preparation method of the present invention can obtain a diameter of major diameter synthetic ruby.
Description
Technical field
The invention belongs to the preparation method technical field of artificial intraocular lensess, more particularly to a kind of synthetic major diameter ruby
Method.
Background technology
Traditional general alumina powder in process of production, is the toner for solving the problems, such as alumina powder, all can be in aluminum sulfate
The melting of ammonium raw material roasting powder adds some chemical impurities (such as in vivo：Chromium oxide etc.).Synthetic ruby production at present
Producer, is all that the alumina powder of the above-mentioned addition chemical impurity for adopting is produced.Traditional processing technology include additive color agent raw material,
Slotting crystal seed, sintering crystal step, sintering crystal are divided into material crystallization, center, crystal pulling root, crystal are expanded and isodiametric growth, tool
Body：Using toner α-Al2O3It is alumina powder jointed as raw material, crystal seed is 62 ° of crystal orientation of 68 ° of crystal orientation of M axles or A axles, oxyhydrogen ratio
1.8～2.2:1,2030～2080 DEG C of flame thermal field grows total time 8h, with single crystal growth diameter obtained in the manufacturing process
Less, major part existsIt is less able to reachMajor diameter ruby above, processing and utilization rate
It is low, it is relatively costly；Therefore extensive application of the ruby in fields such as industry, electronics, jewelry decorative kinds is limit always.
The content of the invention
Technical problem solved by the invention is to provide a kind of evenness, improves effective rate of utilization, reduces production cost
The ruby preparation method of synthetic major diameter.
The ruby preparation method of artificial synthesizing large diameter of the invention, comprises the steps：
A, addition raw material：Add raw materials in screen cloth charging hopper, addition for screen cloth charging hopper 2/3；
B, slotting crystal seed；
C, igniting：Light oxyhydrogen；
D, sintering crystal；
Wherein, step D sintering crystal includes procedure below：
(1) material crystallization：Tap screen cloth charging hopper blanking；
(2) to center：While material is crystallized, with the projection alignment flame high temperature center of fast speed movement growth with
Material center, is melted crystal seed top, receives powder in crystalline state；
(3) crystal expands：Tap screen cloth charging hopper blanking, control drip dimension oxygen speed expand crystal, degrowth speed
10～20mm/h of degree；
(4) isodiametric growth：Tap screen cloth charging hopper blanking, control drip dimension oxygen speed expand crystal, degrowth speed
Spend for 25～40mm/h；
E, blowing out cooling：Stop blanking, supply oxyhydrogen, after cooling, obtain final product crystal.
In above-mentioned technical proposal, raw material described in step A be aluminium oxide toner powder, purity be at least 99.998%, particle diameter
4.1 μm～8.7 μm, 1.34～1.86g/m of density3.Aluminium oxide toner powder is produced with aluminium hydroxide purification, is not substantially deposited
In the destruction to large natural environment, the content of its impurity will not cause direct shadow to the quality of synthetic ruby crystals body
Ring.
In above-mentioned technical proposal, the preferred α-Al of the raw material2O3Toner powder.
In above-mentioned technical proposal, the sieve number of screen cloth charging hopper described in step A is 60～120 mesh.
In above-mentioned technical proposal, the crystal seed that crystal seed adopts 68 ° of crystal orientation of M axles or 62 ° of crystal orientation of A axles described in step B, is inserted；It is preferred that A
The crystal seed of 62 ° of crystal orientation of axle.During from crystal seed, the molten brilliant termination of crystal seed need to be for four directions four just, it is impossible to have the crystal orientation number of degrees and crackle to lack
Fall into, otherwise its light refraction can be produced affects and crystal cleavage quality problems.
In above-mentioned technical proposal, the flame thermal field that the igniting of step C is adopted is set as 2200～2500 DEG C, preferred flame thermal field
For 2400 DEG C, the hydrogen-oxygen mol ratio of flame is 1.8～2.2:1.This is because crystal to the thermal field of oxyhydrogen flame in sintering furnace compared with
For sensitivity, thermal field frequently occurs fluctuation, crystal sudden contraction can be caused, expand or it is serious superfuse, so as to affect the quality of product
With profile quality；Toner impurity content in raw material is higher, causes raw material powder particles fusing point higher.
In above-mentioned technical proposal, need to control the amount of dropping material during step D sintering crystal, to make the molten of crystalline solid
Melting layer is more preferably crystallized.Therefore step D sintering crystal controls the amount of dropping material by tapping screen cloth charging hopper, single taps blanking amount and is
1.8～2.2g.Simultaneously, it is impossible to quickly tap blanking, it is impossible to continue blanking, can otherwise produce powder fusing impermeable, cause crystallization
Half-cooked quality problems, therefore control dropping material taps 18～25 beats/min of frequency.In step D sintering crystal, further control：
(1) material crystallization：It is 18～25 beats/min that blanking taps frequency, and single taps blanking 0.8～1.2g of amount.
(2) to center：While material is crystallized, with the projection alignment flame high temperature center of fast speed movement growth with
Material center, is melted crystal seed top, receives powder in crystalline state.
(3) crystal expands：Dimension oxygen speed of dripping is 1～3 second/drop；Oxygen flow is controlled for 10～18m3Adjustment drop after/H
Water dimension oxygen speed is 3～10 seconds/drop；It is 20～30 beats/min that blanking taps frequency, and single taps blanking 1.2～1.8g of amount.
(4) isodiametric growth：Dimension oxygen speed of dripping is 12～18 seconds/drop；Oxygen flow is constant about：20±5m3/H；Fall
It is 50～60 beats/min that material taps frequency, only secondary percussion blanking 1.8～2.2g of amount.
In above-mentioned technical proposal, step E cool time is 40-60min.
Beneficial effects of the present invention are as follows：
1) compared with traditional processing technology, the toner impurity content in the raw material adopted due to traditional handicraft is higher, causes
Raw material powder particles fusing point is higher, crystalline solid internal stress expand, so cannot synthetic major diameter ruby, its diameter model
Enclose onlyAnd preparation method of the present invention can be obtainedThe synthetic of major diameter is red
Gem.
2) it is 92% on aluminium oxide toner powder Commercial cultivation rate theory, but the utilization rate of preparation method of the present invention is actually
It is 98%, greatly improves labor productivity, reduces production cost.
3) as the granule fusing point of aluminium oxide toner powder is higher, for improve production efficiency, improve flame thermal field
2200～2500 DEG C of molten brilliant temperature is reached, is made artificial synthetic ruby breach the little difficulty of traditional handicraft finished diameter, is obtained
Arrive a diameter ofMajor diameter synthetic ruby.
Specific embodiment
The specific embodiment of form, remakes further specifically to the above of the present invention by the following examples
It is bright, illustrate but do not limit the present invention.Preparation method of the present invention includes A, addition raw material：B, slotting crystal seed；C, igniting；D, sinter
Body；E, blowing out cool down five big steps.Wherein：D, sintering crystal include that (1) material is crystallized：(2) to center；(3) crystal expands
(4) four operating procedures of isodiametric growth.Specific preparation method of the present invention is prepared using sintering furnace, with α-Al2O3Color
Agent powder prepares the ruby technological process of synthetic major diameter for raw material and is specially：Addition raw material → insert a crystal seed → hydrogen-oxygen
Flame sinters → clears up sintering furnace → material and crystallizes → center → crystal expansion → isodiametric growth → blowing out is cooled down → taking-up list
Crystal, specially：
1st, add raw material：α-Al2O3Toner powder is poured in 60～120 eye mesh screen charging hoppers, adds a cover isolation dust.By
Larger in toner powder proportion, self gravitation is easily compacted powder, it is impossible to effectively loose blanking, so addition is to install hopper additional
2/3；
2nd, insert crystal seed：In candlestick top end, the crystal seed of 62 ° of crystal orientation of A axles is inserted perpendicularly into；During from crystal seed, the molten crystalline substance of crystal seed
Termination need to be for four directions four just, it is impossible to have the crystal orientation number of degrees and crack defect, otherwise impact can be produced on its light refraction and crystal is held
Split quality problems.
3rd, put oxyhydrogen flame：Hydrogen-oxygen gas flame is lighted, flame thermal field set point is at 2200 DEG C～2500 DEG C；Due to flame
The change of thermal field, the hydrogen-oxygen mol ratio for adjusting flame are 1.8～2.2:1.
4th, clear up sintering furnace：With dedicated cleaning tool, the gently moving around the inboard wall of burner hearth makes the impurity such as the powder of bonding
Drop；
5th, material crystallization：Start to rotate and tap bar, tapping hopper guide bar carries out blanking, crystallizes on crystal seed top；Fall
Material taps 18～25 beats/min of frequency, and single taps blanking 0.8～1.2g of amount；
6th, to center：While material is crystallized, with the projection alignment flame high temperature center of fast speed movement growth with
Material center, is melted crystal seed top, receives powder in crystalline state.
7th, crystal expands：Control is dripped and ties up oxygen speed, increases oxygen flow, and oxygen flow is：10～18m3/H.According to crystalline substance
Bulk-growth state, controls effective cooperation of discharge quantity and degrowth speed；Dimension oxygen speed of dripping is 1～3 second/drop；Control oxygen
Throughput is 10～18m3After/H, dimension oxygen speed of dripping is adjusted from fast to slow：3～10 seconds/drop；Dropping material taps frequency：20～
30 beats/min；Single taps blanking 1.2～1.8g of amount；Degrowth 10～20mm/h of speed；
8th, isodiametric growth：The control of frequency, drip dimension oxygen speed is tapped to degrowth speed, dropping material mainly；It is brilliant
When body is normal isometrical, degrowth speed：25～40mm/h；Dropping material taps frequency：50～60 beats/min；Single blanking amount
1.8～2.2g；Dimension of dripping oxygen speed：12～18 seconds/drop；Oxygen flow is constant about：20±5m3/H。
9th, blowing out cooling：Close hydrogen-oxygen air valve；Crystal cool time is 40～60min；
10th, take out crystal：Require without special process.
Following examples be carry out under the guidance of above-mentioned technological process be embodied as preparation example.
Embodiment 1
Prepare：With sintering machine as production equipment；Raw material is α-Al2O3Toner powder, purity are 99.998%, mean diameter
For 6.3 μm.The screen cloth of charging hopper is 80 mesh.
Cleaning：Inside aerator purging charging hopper.
Charging：α-Al2O3Toner powder is poured in 80 eye mesh screen charging hoppers, adds a cover isolation dust.
Slotting crystal seed：The crystal seed of 62 ° of crystal orientation of A axles is inserted perpendicularly into the projection top end of growth.
Sintering crystal：1), igniting, regulating QI：Hydrogen-oxygen gas flame is lighted, the ratio 1.8 that oxyhydrogen is just commonly using gas is adjusted:1, fire
2200 DEG C of flame thermal field.
2), material crystallization：Start to rotate and tap bar, tapping hopper guide bar carries out blanking, crystallizes on crystal seed top；Fall
Material taps 18～25 beats/min of frequency, and single taps blanking 0.8～1.2g of amount.
3), to center (flame kernel, powder center)：In blanking simultaneously, the growth of slight, quick mobile crystal seed is projection right
Accurate its flame kernel, plate cutting center, so that powder is crystallized at crystal seed upper end.
4), crystal expands：With the dimension oxygen speed of dripping of 1 second 2 drop, oxygenation expansion is carried out.Oxygen flow is 12m3/H.It
Afterwards, dimension of dripping oxygen speed is changed into：3～10 seconds/drop；Dropping material taps frequency：20～30 beats/min；Single taps blanking amount 1.2
～1.8g；Degrowth 10～20mm/h of speed；Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal
The time required to expanding, control is within 30min.
5), isodiametric growth：Slow down dimension oxygen speed of dripping to 12～18 seconds/drop, improve dropping material and frequency is tapped to 50～60
Secondary/min, single blanking 1.8～2.2g of amount；Accelerate degrowth speed to 25～40mm/h；Crystal is made to become in micro- expansion upwards
Gesture grows.2200 DEG C of oxyhydrogen flame kernel temperature.It is 5h the time required to whole isodiametric growth process.
6), blowing out cooling：Stop blanking, close hydrogen-oxygen air valve, stop declining；Crystal is taken out after non-shock chilling.Crystal
Cool time is 40min.
The crystal for obtaining does not split, and stands intact, diameter ф 26-28mm, total length 127mm.
The appraising datum of crystal is as follows：
Main component：Al2O3, belong to trigonal system；Fusing point：Crystalline melt temperatures are 2300 DEG C；Density：3.97g/cm3-
4.10g/cm3；Hardness of crystals：9 grades of Mohs；
Crystal color：Pink melts impurity invariably to peony；Split surface flat smooth, gloss：It is translucent, glass light
Pool, adamantine luster；Index of refraction：1.76-1.77；Birefringence：0.008-0.010
Crystal mass index：Qualification rate more than 85%.
Embodiment 2
Prepare：With sintering machine as production equipment；Raw material is α-Al2O3Toner powder, purity are 99.998%, mean diameter
For 6.3 μm.The screen cloth of charging hopper is 80 mesh.
Cleaning：Inside aerator purging charging hopper.
Charging：α-Al2O3Toner powder is poured in 80 eye mesh screen charging hoppers, adds a cover isolation dust.
Slotting crystal seed：The crystal seed of 68 ° of crystal orientation of M axles is inserted perpendicularly into the projection top end of growth.Sintering crystal：1), igniting, tune
Gas：Hydrogen-oxygen gas flame is lighted, the ratio 2.0 that oxyhydrogen is just commonly using gas is adjusted:1,2300 DEG C of flame thermal field.
2), material crystallization：Start to rotate and tap bar, tapping hopper guide bar carries out blanking, crystallizes on crystal seed top；Fall
Material taps 18～25 beats/min of frequency, and single taps blanking 0.8～1.2g of amount.
3), to center (flame kernel, powder center)：In blanking simultaneously, slight, quick mobile growth is projection to be directed at its fire
Flame center, plate cutting center, so that powder is crystallized at crystal seed upper end.
4), crystal expands：The dimension oxygen speed of dripping of 1 second 2 drop, carries out oxygenation expansion.Oxygen flow is 14m3/H.It
Afterwards, dimension of dripping oxygen speed is changed into：3 seconds～10 seconds/drop；Dropping material taps frequency：20～30 beats/min；Single taps blanking amount
1.2～1.8g；Degrowth 10～20mm/h of speed；Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.It is whole brilliant
Body is controlled within 40min the time required to expanding.
5), isodiametric growth：Slow down dimension oxygen speed of dripping to 12～18 seconds/drop, improve dropping material and frequency is tapped to 50～60
Secondary/min, single blanking 1.8～2.2g of amount；Accelerate degrowth speed to 20～35mm/h；Crystal is made to become in micro- expansion upwards
Gesture grows.2300 DEG C of oxyhydrogen flame kernel temperature.It is 4.5h the time required to whole isodiametric growth process.
6), blowing out cooling：Stop blanking, close hydrogen-oxygen air valve, stop declining；Crystal is taken out after non-shock chilling.Crystal
Cool time is 40min.
The crystal for obtaining does not split, and stands intact, diameter ф 30-32mm, total length 115mm.
The appraising datum of crystal is as follows：
Main component：Al2O3, belong to trigonal system；Fusing point：Crystalline melt temperatures are 2300 DEG C；Density：3.97g/cm3-
4.10g/cm3；Hardness of crystals：9 grades of Mohs；
Crystal color：Pink melts impurity invariably to peony；Split surface flat smooth, gloss：It is translucent, glass light
Pool, adamantine luster；Index of refraction：1.76-1.77；Birefringence：0.008-0.010
Crystal mass index：Qualification rate more than 85%.
Embodiment 3
Prepare：With sintering machine as production equipment；Raw material is α-Al2O3Toner powder, purity are 99.998%, mean diameter
For 5.3 μm.The screen cloth of charging hopper is 80 mesh.
Cleaning：Inside aerator purging charging hopper.
Charging：α-Al2O3Toner powder is poured in 80 eye mesh screen charging hoppers, adds a cover isolation dust.
Slotting crystal seed：The crystal seed of 68 ° of crystal orientation of M axles is inserted perpendicularly into the projection top end of growth.
Sintering crystal：1), igniting, regulating QI：Hydrogen-oxygen gas flame is lighted, the ratio 2.2 that oxyhydrogen is just commonly using gas is adjusted:1, fire
2400 DEG C of flame thermal field.
2), material crystallization：Start to rotate and tap bar, tapping hopper guide bar carries out blanking, crystallizes on crystal seed top；Fall
Material taps 18～25 beats/min of frequency, and single taps blanking 0.8～1.2g of amount.
3), to center (flame kernel, powder center)：In blanking simultaneously, slight, quick mobile growth is projection to be directed at its fire
Flame center, plate cutting center, so that powder is crystallized at crystal seed upper end.
4), crystal expands：The dimension oxygen speed of dripping of 1 second 2 drop, carries out oxygenation expansion.Oxygen flow is 16m3/H.It
Afterwards, dimension of dripping oxygen speed is changed into：3 seconds～10 seconds/drop；Dropping material taps frequency：20～30 beats/min；Single taps blanking amount
1.2～1.8g；Degrowth 10～20mm/h of speed；Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.It is whole brilliant
Body is controlled within 60min the time required to expanding.
5), isodiametric growth：Slow down dimension oxygen speed of dripping to 12～18 seconds/drop, improve dropping material and frequency is tapped to 50～60
Secondary/min, single blanking 1.8～2.2g of amount；Accelerate degrowth speed to 20～30mm/h；Crystal is made to become in micro- expansion upwards
Gesture grows.2400 DEG C of oxyhydrogen flame kernel temperature.It is 4h the time required to whole isodiametric growth process.
6), blowing out cooling：Stop blanking, close hydrogen-oxygen air valve, stop declining；Crystal is taken out after non-shock chilling.Crystal
Cool time is 60min.
The crystal for obtaining does not split, and stands intact, diameter ф 31-33mm, total length 110mm.
The appraising datum of crystal is as follows：
Main component：Al2O3, belong to trigonal system；Fusing point：Crystalline melt temperatures are 2300 DEG C；Density：3.97g/cm3-
4.10g/cm3；Hardness of crystals：9 grades of Mohs；
Crystal color：Pink melts impurity invariably to peony；Split surface flat smooth, gloss：It is translucent, glass light
Pool, adamantine luster；Index of refraction：1.76-1.77；Birefringence：0.008-0.010
Crystal mass index：Qualification rate more than 80%.
Embodiment 4
Prepare：With sintering machine as production equipment；Raw material is α-Al2O3Toner powder, purity are 99.998%, mean diameter
For 4.6 μm.The screen cloth of charging hopper is 80 mesh.
Cleaning：Inside aerator purging charging hopper.
Charging：α-Al2O3Toner powder is poured in 80 eye mesh screen charging hoppers, adds a cover isolation dust.
Slotting crystal seed：The crystal seed of 62 ° of crystal orientation of A axles is inserted perpendicularly into the projection top end of growth.
Sintering crystal：1), igniting, regulating QI：Hydrogen-oxygen gas flame is lighted, the ratio 2.0 that oxyhydrogen is just commonly using gas is adjusted:1, fire
2400 DEG C of flame thermal field.
2), material crystallization：Start to rotate and tap bar, tapping hopper guide bar carries out blanking, crystallizes on crystal seed top；Fall
Material taps 18～25 beats/min of frequency, and single taps blanking 0.8～1.2g of amount.
3), to center (flame kernel, powder center)：In blanking simultaneously, slight, quick mobile growth is projection to be directed at its fire
Flame center, plate cutting center, so that powder is crystallized at crystal seed upper end.
4), crystal expands：The dimension oxygen speed of dripping of 1 second 2 drop, carries out oxygenation expansion, and oxygen flow is 18m3/H.It
Afterwards, dimension of dripping oxygen speed is changed into：1 second～8 seconds/drop；Dropping material taps frequency：20～30 beats/min；Single taps blanking amount
1.2～1.8g；Degrowth 10～20mm/h of speed；Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.It is whole brilliant
Body is controlled within 90min the time required to expanding.
5), isodiametric growth：Slow down dimension oxygen speed of dripping to 12～18 seconds/drop, improve dropping material and frequency is tapped to 50～60
Secondary/min, single blanking 1.8～2.2g of amount；Accelerate degrowth speed to 20～30mm/h；Crystal is made to become in micro- expansion upwards
Gesture grows.2400 DEG C of oxyhydrogen flame kernel temperature.It is 3.5h the time required to whole isodiametric growth process.
6), blowing out cooling：Stop blanking, close hydrogen-oxygen air valve, stop declining；Crystal is taken out after non-shock chilling.Crystal
Cool time is 60min.
The crystal for obtaining does not split, and stands intact, diameter ф 33-36mm, total length 93mm.
The appraising datum of crystal is as follows：
Main component：Al2O3, belong to trigonal system；Fusing point：Crystalline melt temperatures are 2300 DEG C；Density：3.97g/cm3-
4.10g/cm3；Hardness of crystals：9 grades of Mohs；
Crystal color：Pink melts impurity invariably to peony；Split surface flat smooth, gloss：It is translucent, glass light
Pool, adamantine luster；Index of refraction：1.76-1.77；Birefringence：0.008-0.010
Crystal mass index：Qualification rate more than 80%.
As seen from the above-described embodiment, can obtain a diameter of using preparation method of the present inventionIt is big straight
Footpath synthetic ruby.
Claims (10)
1. the ruby preparation method of synthetic major diameter, it is characterised in that：Comprise the steps：
A, addition raw material：Add raw materials in screen cloth charging hopper, addition for screen cloth charging hopper 2/3；
B, slotting crystal seed；
C, igniting：Light oxyhydrogen；
D, sintering crystal；
Wherein, step D sintering crystal includes procedure below：
(1) material crystallization：Tap screen cloth charging hopper blanking；
(2) to center：While material is crystallized, with the projection alignment flame high temperature center of fast speed movement growth and blanking
The heart, is melted crystal seed top, receives powder in crystalline state；
(3) crystal expands：Tap screen cloth charging hopper blanking, control drip dimension oxygen speed expand crystal, degrowth speed 10
～20mm/h；
(4) isodiametric growth：Tap screen cloth charging hopper blanking, control drip dimension oxygen speed expand crystal, degrowth speed is
25～40mm/h；
E, blowing out cooling：Stop blanking, supply oxyhydrogen, after cooling, obtain final product crystal.
2. the ruby preparation method of synthetic major diameter according to claim 1, it is characterised in that：Described in step A
Raw material be aluminium oxide toner powder, purity be at least 99.998%, 4.1 μm～8.7 μm of particle diameter, 1.34～1.86g/m of density3。
3. the ruby preparation method of synthetic major diameter according to claim 2, it is characterised in that：Described in step A
Aluminium oxide toner powder is α-Al2O3Toner powder.
4. the ruby preparation method of synthetic major diameter according to claim 1, it is characterised in that：Described in step A
The sieve number of screen cloth charging hopper is 60～120 mesh.
5. the ruby preparation method of synthetic major diameter according to claim 1, it is characterised in that：Described in step B
Slotting crystal seed adopts the crystal seed of 68 ° of crystal orientation of M axles or 62 ° of crystal orientation of A axles；It is preferred that the crystal seed of 62 ° of crystal orientation of A axles.
6. the ruby preparation method of synthetic major diameter according to claim 1, it is characterised in that：Step C is lighted a fire
Using flame thermal field be set as 2200～2500 DEG C, preferred flame thermal field be 2400 DEG C.
7. the ruby preparation method of synthetic major diameter according to claim 1, it is characterised in that：Step C flame
Hydrogen-oxygen mol ratio be 1.8～2.2:1.
8. the ruby preparation method of synthetic major diameter according to claim 1, it is characterised in that：Step D is sintered
Crystal controls the amount of dropping material by tapping screen cloth charging hopper, and it is 1.8～2.2g that single taps blanking amount；Dropping material taps frequency
18～25 beats/min.
9. the ruby preparation method of synthetic major diameter according to claim 1, it is characterised in that：Step D is sintered
In crystal, following any one is at least met：
(1) material crystallization：It is 18～25 beats/min that blanking taps frequency, and single taps blanking 0.8～1.2g of amount；
(2) to center：While material is crystallized, with the projection alignment flame high temperature center of fast speed movement growth and blanking
The heart, is melted crystal seed top, receives powder in crystalline state；
(3) crystal expands：Dimension oxygen speed of dripping is 1～3 second/drop；Oxygen flow is controlled for 10～18m3The dimension oxygen that drips is adjusted after/H
Speed is 3～10 seconds/drop；It is 20～30 beats/min that blanking taps frequency, and single taps blanking 1.2～1.8g of amount；
(4) isodiametric growth：Dimension oxygen speed of dripping is 12～18 seconds/drop；Oxygen flow is constant about：20±25m3/H；Dropping material strikes
Frequency is hit for 50～60 beats/min, only secondary percussion blanking 1.8～2.2g of amount.
10. the ruby preparation method of synthetic major diameter according to claim 1, it is characterised in that：Step E is cooled down
Time is 40-60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710053444.5A CN106544730A (en) | 2017-01-22 | 2017-01-22 | A kind of ruby preparation method of synthetic major diameter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710053444.5A CN106544730A (en) | 2017-01-22 | 2017-01-22 | A kind of ruby preparation method of synthetic major diameter |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106544730A true CN106544730A (en) | 2017-03-29 |
Family
ID=58398411
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710053444.5A Pending CN106544730A (en) | 2017-01-22 | 2017-01-22 | A kind of ruby preparation method of synthetic major diameter |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106544730A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942698A (en) * | 2010-09-28 | 2011-01-12 | 四川鑫通新材料有限责任公司 | Preparation method for alpha-aluminium oxide monocrystal |
| CN102011185A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Method for artificially synthesizing sapphire |
| CN102011184A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| CN102021647A (en) * | 2010-10-22 | 2011-04-20 | 北京工业大学 | Method for rapid growth of centimeter magnitude ruby crystal |
| CN103882521A (en) * | 2014-04-04 | 2014-06-25 | 玉溪市明珠晶体材料有限公司 | Method for growing jewelry-grade ruby monocrystal |
-
2017
- 2017-01-22 CN CN201710053444.5A patent/CN106544730A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942698A (en) * | 2010-09-28 | 2011-01-12 | 四川鑫通新材料有限责任公司 | Preparation method for alpha-aluminium oxide monocrystal |
| CN102021647A (en) * | 2010-10-22 | 2011-04-20 | 北京工业大学 | Method for rapid growth of centimeter magnitude ruby crystal |
| CN102011185A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Method for artificially synthesizing sapphire |
| CN102011184A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| CN103882521A (en) * | 2014-04-04 | 2014-06-25 | 玉溪市明珠晶体材料有限公司 | Method for growing jewelry-grade ruby monocrystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102162130B (en) | Preparation method of sapphire monocrystalline | |
| CN106319620B (en) | A kind of crystal pulling method of pulling of crystals | |
| CN108203844B (en) | Magnesium tantalate series crystal and its preparing process | |
| CN105936584B (en) | A kind of preparation method of quartz glass | |
| CN107236992B (en) | A kind of flame melt method growing optics-level strontium titanate monocrystal body device | |
| CN107130289A (en) | A kind of growing method for improving heat exchange large size sapphire crystal | |
| CN104131339A (en) | Preparation method of polysilicon chip | |
| US20100139549A1 (en) | Quartz Glass Crucible for Pulling Silicon Single Crystal and Method of Manufacturing Quartz Glass Crucible for Pulling Silicon Single Crystal | |
| CN107858751A (en) | A kind of crystal pulling method for improving pulling of crystals method crystal forming rate | |
| KR100753322B1 (en) | Method and apparatus for preparing crystal | |
| CN106319621A (en) | Large-size czochralski silicon single crystal growth method | |
| CN102011184B (en) | Production method of alpha-aluminum oxide single crystal | |
| JP2008508187A (en) | Method for growing a single crystal from a melt | |
| CN104790034B (en) | A kind of method for preparing aluminum oxide polycrystal body | |
| CN106544730A (en) | A kind of ruby preparation method of synthetic major diameter | |
| CN103205799A (en) | Method for growing C-oriented white stone crystals | |
| JP5855293B2 (en) | Method for producing silica glass crucible | |
| CN102011185B (en) | Method for artificially synthesizing sapphire | |
| CN106149048B (en) | A kind of KY method sapphire low vacuum growing method | |
| CN101956231A (en) | Quartz glass crucible and preparation method thereof | |
| CN106987903B (en) | A kind of improved large scale synthetic sapphire production technology | |
| CN107805840A (en) | A kind of crystal pulling mechanism of crystal pulling furnace | |
| CN207244047U (en) | A kind of high density sapphire crystal quick process units of high purity aluminium oxide crystal block | |
| CN104790035A (en) | Method for growing red aluminum oxide gemstone single crystal | |
| CN209144302U (en) | Flame melt method crystal growing furnace furnace structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170329 |