CN1003459B - Method for growing of colour crystal - Google Patents
Method for growing of colour crystal Download PDFInfo
- Publication number
- CN1003459B CN1003459B CN86101506.1A CN86101506A CN1003459B CN 1003459 B CN1003459 B CN 1003459B CN 86101506 A CN86101506 A CN 86101506A CN 1003459 B CN1003459 B CN 1003459B
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- growth
- crystal
- koh
- naoh
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Abstract
The present invention relates to a growing method of color crystals, which adopts NaOH-KOH solvents and selects favorable cut types (+Y,-Y, (30 to 80 degrees)X cutting) according to the crystallizing habits of crystals, and ions (Al<3+>, CO<2>, Fe<3+>, Mn<4+]>) are properly doped. The growing method is carried out in a high-pressure vessel under the atmospheric pressure of 1200 to 1600 at the growth temperature of 335 to 360 DEG C, and a temperature difference is from 15 to 25 DEG C. High-quality color crystals having the advantages of uniform color formation, high yield, no cotton, no crystal twins, no cracks, no gas bubbles, etc. can grow, which is suitable for practical application.
Description
Involved in the present invention is growing method, particularly utilize in the NaOH-KOH mixed solvent, employing+Y ,-seed crystal of Y, (the 30-80 degree is cut) and X cut type is with " the terraced method of hydro-thermal temperature " the grow method of citrite (smoky quartz).
Citrite is a kind of of colour crystal, and it is a kind of ideal material of making the yellow quartz mirror; Also can be used for many new technical field, the protection of the incandescence that sends in protection, other technical field such as the smelting iron and steel as the incandescence that rocket, guided missile sent.China northeast and northwest drought and desert region need a large amount of citrite glasses, (estimate annual about 30-50 ton.）
In the past, citrite was that mineral crystal makes behind gamma-ray irradiation.Because mineral crystal extremely lacks, supply falls short of demand; In addition, the mineral crystal defective is many, and cotton, inclusion, twin crystal, crackle etc. are arranged, and irradiation institute quality is inhomogeneous, so need carry out synthetic.
The method of existing synthetic citrite can be divided into two kinds substantially:
First kind: during growing crystal, be to adopt in yellow soda ash (or salt of wormwood) solvent, to add dopant ion (FeCO
3, MnCO
3, CoCO
3 ) formation ion look.(" crystallization engineering " 984,1971; Adopt the synthetic " piezoquartz technology " 1984 of look crystal.4; " artificial lens " 1985.Vol14 № 2).But in above-mentioned solvent, the crystal of being grown, quality is inhomogeneous, and the also difficult control of color.Its growth technique is also stable inadequately, and there is the crack in the growth later stage, and crystalline state is bad, and it is slow to grow up, poor repeatability.
Second kind: be in single NaOH solvent, to add Al
3+, the crystal of being grown shows dark brown behind gamma-ray irradiation.(Kristallografiya Vol.12 № 165-9(1967) Phys, stat.Sol.(a) 29,659(1975), this is studied mainly from Al
3+Colour center effect in crystal is set out, and inquires into the formation of dark brown crystalline substance (smoky quartz), has at length studied crystalline spectral line of absorption and Al
3+The mechanism that colour center forms.But cut type and quality homogeneity to the speed in the crystal growth, seed crystal there is no report.
Common a kind of cranberry glass on the market, its hardness low (Mohs' hardness is 5), not anti-windsand mill corrosion is made dark brown glasses, and the smooth finish life-span is long not as good as quartzy.
Purpose of the present invention is to provide a kind of citrite that is used to make dark brown glasses (smoky quartz) growth method of market in urgent need.The feature of this method is: (1) adopts NaOH-KOH mixed base solvent.(2) seed crystal need edge+Y ,-the Y(30-80 degree) and the X cut type make crystal growth rate fast, quality is even, the crystal growth size is easy to control, cost is low.
Technology contents of the present invention is as follows:
One, the pre-treatment of raw material:
Adopt 3-4 level smelting quartz and vein quartz, wash, and, clean, dry with distilled water again with salt acid soak 24 hours, stand-by.
Two, the preparation of growth solution:
Adopt NaOH(1-1.5N), KOH(0.3-0.8N) be made into mixed solvent, add main dopant ion Al
3+(weight %, as follows) 0.1-0.5%; Also can be according to the needs of color, select to add different ions: blueness adds Co
2+0.1-0.5%; The yellow Fe of lemon
2+0.1-0.3%; Purple adds Fe
3+(solvent NaCl) 0.1-0.5%; Blackish green Mn
4+0.1-0.6%.
Three, seed crystal cut type and pre-treatment:
Cut type+Y 30-80 degree or,
-Y 30-80 degree or,
X cuts
Seed crystal thickness is 2 millimeters.With ultrasonic drilling (or drill bit punching).
Seed crystal is washed, put into washing lotion again and soaked 24 hours, wash, stand-by.
Seed crystal after cleaning is worn with iron wire and to be tied on the seed crystal frame.
Four, crystalline growth:
It is to have the seed crystal frame of seed crystal to pack in the still that the stand-by quartz raw material of oven dry is packed in the vertical autoclave.Pour the mixed base solvent for preparing into, and measure the height of liquid level in the still, compactedness is the relative still volume of 80-83%().Autoclave packed into heat, heat in the holding furnace.
Growth temperature is controlled at 335-365 ℃
Temperature difference 15-25 ℃
Pressure 1200-1600 normal atmosphere
Growth velocity 0.6-1.3 millimeter/sky
Five, crystalline irradiation:
Behind the growth ending, take out crystal Co
60Irradiation, dosage is: 1 * 10
5-10
7Rad.
Effect of the present invention is: owing to adopted preferential orientation and mixed base (NaOH-KOH) solvent that meets Growth Habit, make crystal growth rate improve 30-40%; Owing to controlled adulterated distribution, through Co
60Irradiation, gained crystal quality is even, and reaching does not have cotton, and no twin crystal, crackle and bubble etc. meet the requirement of making the yellow quartz mirror fully.
Below with tabular form effect of the present invention is described:
Citrite is durable in use and graceful luxurious, more is applicable to make dark brown glasses.
Performance of the present invention describes by table four.
Table four has been listed the growth performance of citrite, and the effect that is reached under each condition.
Table five has been listed adulterated ionic species of colour crystal and concentration range performance.
The enforcement of table four, citrite growth
Claims (24)
1, a kind of hydrothermal method adopts NaOH, KOH to make solvent, with Al, Fe, Co, Mn ion do twoly to mix, three doping agents of mixing, adopt X or+Y or-growth of Y seed crystal cut type, use Co irradiation again, (dosage is 10
5-10
7Rad) colour crystal growth technique,
Comprise: growth temperature 335-365 ℃
Temperature difference 15-25 ℃
Pressure 1200-1600 normal atmosphere,
It is characterized by the seed crystal cut type and be ± Y50 °.
2, according to the method for claim 1, it is characterized in that:
Selected dopant ion and concentration range thereof are as follows: (weight %)
A, growth selected ion of citrite and concentration range thereof:
Al
3+0.1-0.5
Co
2+0.2-0.3
Fe
3+0.01;
B, growth purple crystal is mixed Fe
30.1-0.7
Blue crystal Co
2+0.1-0.4
Lemon yellow Fe
2+0.1-0.6
Blackish green Mn
4+0.2-0.5
3, according to the method for claim 1, it is characterized in that:
A, used NaOH, KOH are the mixed base solvent;
B, its concentration range: KOH 0.3-0.8N
NaOH 1.0-1.5N。
4, according to the method for claim 1 or 3, it is characterized in that:
The growth colour crystal need add following solvent:
Purple adds NaCl
The lemon yellow K that adds
2CO
3
The blackish green K that adds
2CO
3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86101506.1A CN1003459B (en) | 1986-06-27 | 1986-06-27 | Method for growing of colour crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86101506.1A CN1003459B (en) | 1986-06-27 | 1986-06-27 | Method for growing of colour crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86101506A CN86101506A (en) | 1988-01-06 |
| CN1003459B true CN1003459B (en) | 1989-03-01 |
Family
ID=4801413
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86101506.1A Expired CN1003459B (en) | 1986-06-27 | 1986-06-27 | Method for growing of colour crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1003459B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102367199B (en) * | 2011-10-08 | 2013-06-05 | 浙江伟兴水晶有限公司 | Preparation method of lilac crystal bead stock |
| CN102372432B (en) * | 2011-10-08 | 2013-07-17 | 浙江伟兴水晶有限公司 | Preparation method of dark blue crystal ball blank |
| CN102372433B (en) * | 2011-10-08 | 2013-10-30 | 浙江伟兴水晶有限公司 | Preparation method of yellow crystal ball blank |
| CN103938264A (en) * | 2014-04-29 | 2014-07-23 | 三明市港乐水晶电子有限公司 | Method for growing optical crystal |
-
1986
- 1986-06-27 CN CN86101506.1A patent/CN1003459B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN86101506A (en) | 1988-01-06 |
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