CN107604441A - A kind of dual temperature area method crystal growing apparatus and DAST crystal growth techniques - Google Patents
A kind of dual temperature area method crystal growing apparatus and DAST crystal growth techniques Download PDFInfo
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- CN107604441A CN107604441A CN201710816696.9A CN201710816696A CN107604441A CN 107604441 A CN107604441 A CN 107604441A CN 201710816696 A CN201710816696 A CN 201710816696A CN 107604441 A CN107604441 A CN 107604441A
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Abstract
The invention discloses a kind of dual temperature area method crystal growing apparatus and DAST crystal growth techniques.Dual temperature area method crystal growing apparatus top is low-temperature space, has cup-shaped sandwich；Bottom is high-temperature region, in ball bottle-shaped；Connected between upper and lower warm area by straight tube, and be furnished with thermal baffle.Excessive DAST sources powder forms high temperature saturated solution in bottom high-temperature region, is transmitted by connecting straight tube to top low-temperature space, forms supersaturated solution after being cooled down by top low-temperature space, driving force is provided for DAST crystal growths.Dual temperature area method crystal growing apparatus is simple in construction for this, is easy to establishment, is easy to operation.Dual temperature area method DAST crystal growth techniques can avoid influence of the spontaneous nucleation to crystal growing process, realize that DAST crystalcheckeds grow, and be advantageous to improve crystal mass.
Description
Technical field
The present invention relates to a kind of dual temperature area method crystal growing apparatus and DAST（4-N, TMSDMA N dimethylamine base -4 '-N '-methyl -
Azepine stilbene tosilate）The growth technique of crystal.
Background technology
Organic non linear optical material is because its nonlinear optical coefficients is big, fast response time, optic damage threshold value are high, is situated between
Electric constant is low, is easy to the advantages that progress MOLECULE DESIGN, enjoys the researcher concern of the field such as chemistry, crystallography, optics.Its
In, S. R. Marder et al. report the DAST crystal with second-order optical nonlinearity first in August, 1989.DAST is it
English name 4-N, N-dimethylamino-4 '-N '-methyl-stilbazolium tosylate abbreviation, literal translation
Chinese should be 4-N, TMSDMA N dimethylamine base -4 '-N '-methyl-aza stilbene tosilate.Recent study finds DAST
Crystal second order nonlinear coefficient at 1318 nm is 1010 pm/V, electro-optic coefficient is 92 pm/V, can produced at 720 nm
THz wave in the range of 0.1-40 THz, it is widely used in wideband THz wave research field.
But the DAST crystal preparation technology of document report uses aqueous solution cooling method or solution-evaporation, this two major class mostly
Growing method can be influenceed by spontaneous nucleation phenomenon, and the stray crystal of formation can vie each other with seed crystal, reduce the life of seed crystal
Long speed, or even be attached at seed crystal face and trigger seed crystal polymorphic transformation.
The content of the invention
The present invention seeks to overcome in existing DAST crystal growth techniques method spontaneous nucleation to the shadow of crystal growing process
Ring, a kind of dual temperature area method crystal growing apparatus and DAST crystal growth techniques are especially provided.Excessive DAST sources powder is in bottom height
Warm area forms high temperature saturated solution, is transmitted by connecting straight tube to top low-temperature space, is formed and satiated after being cooled down by top low-temperature space
And solution, provide driving force for DAST crystal growths.Dual temperature area method crystal growing apparatus is simple in construction for this, is easy to establishment, just
In operation.Dual temperature area method DAST crystal growth techniques can avoid influence of the spontaneous nucleation to crystal growing process, realize DAST
Crystalchecked grows, and is advantageous to improve crystal mass.
The present invention is achieved by the following technical solutions：A kind of dual temperature area method crystal growing apparatus, it is characterised in that：It is double
Warm area method crystal growing apparatus top is low-temperature space, has cup-shaped sandwich；Wherein, the internal diameter of internal layer cup is 85 ~ 90
Mm, a height of 170 ~ 180 mm, wall thickness are 5 ~ 10 mm；The internal diameter of outer layer cup is 180 ~ 200 mm, is high 140 ~ 150 mm, wall
Thickness is 5 ~ 10 mm；Dual temperature area method crystal growing apparatus bottom is high-temperature region, and in ball bottle-shaped, volume is 25 mL or 50 mL, is used for
Hold excessive solute and form high temperature saturated solution；Upper and lower low-temperature space is connected with high temperature section by straight tube, and straight tube internal diameter is 10 ~
20 mm, a length of 100 ~ 150 mm, wall thickness is 5 ~ 10 mm, and is furnished with thermal baffle, a diameter of 130 ~ 140 mm of thermal baffle, thick
Spend for 5 ~ 10 mm, thermal baffle bottom center 20 mm at pin openings, for heat-insulated and support heat-preservation cotton layer.
One kind of the present invention carries out DAST crystal growth techniques using dual temperature area method crystal growing apparatus, and its feature exists
In：When being used to grow DAST crystal using dual temperature area method crystal growing apparatus, into interlayer, water filling is as heating water bath inner-layer cup
Solution in body, 5-10 g DAST sources powder is added into bottom high-temperature region pin, and inner layer cup is injected at 55-64 DEG C
After DAST- methanol saturated solution 450-850 mL, interior outer cup is sealed by top blind flange；Stroke is entered to upper and lower warm area respectively
Sequence temperature control, the top low-temperature space bath temperature scope after design temperature is stable is 30-39 DEG C, and bottom high-temperature region temperature range is
56-67 ℃；Top low-temperature space reaches set temperature by slow cooling, and rate of temperature fall is 0.05-2.00 DEG C/d, temperature
It is set as temperature constant state after stable；Bottom high-temperature region is set as temperature constant state all the time.
The present invention is molten by the DAST- methanol saturations for suitably adjusting injection different temperatures and volume in R＆D process
The technological parameters such as liquid, top low-temperature space bath temperature, bottom high-temperature region temperature, further stabilize dual temperature area method DAST crystal
Growth technique, therefore invention further provides following preferable dual temperature area method DAST crystal growth techniques.
Currently preferred one kind carries out DAST crystal growth techniques using dual temperature area method crystal growing apparatus, and its feature exists
In：When dual temperature area method crystal growing apparatus is used to grow DAST crystal, into interlayer, water filling is as in heating water bath internal layer cup
Solution, 5-8 g DAST sources powder, the DAST- first that inner layer cup is injected at 55-60 DEG C are added into bottom high-temperature region pin
After alcohol saturated solution 650-850 mL, interior outer cup is sealed by top blind flange；Temperature programmed control is carried out to upper and lower warm area respectively,
Top low-temperature space bath temperature scope after design temperature is stable is 34-39 DEG C, and bottom high-temperature region temperature range is 56-61 DEG C；
Top low-temperature space reaches set temperature by slow cooling, 0.10-1.00 DEG C of rate of temperature fall/d, is set after temperature stabilization
For temperature constant state；Bottom high-temperature region is set as temperature constant state all the time.
The advantages of the present invention are：
（1）A kind of dual temperature area method crystal growing apparatus is provided, suitable for crystal growth from solution process, be particularly suitable for use in solution
The narrower crystal growing process of metastable region scope, it is easy to operate, it is easily controllable.
（2）A kind of dual temperature area method DAST crystal growth techniques are provided, the advantage is that：A. can overcome in solution certainly
Influence of the nucleation to crystal growing process is sent out, the nucleus that spontaneous nucleation is formed can fall into bottom high-temperature region and dissolve again,
It will not be stopped in top low-temperature space and influence the growth of seed crystal；B. up and down after temperature area temperature stabilizing, the concentration of solution point in device
Cloth is also stablized therewith, and seed crystal will be grown with stable growth rate, will not be changed because of the fluctuations of solution concentration, be advantageous to
Improve crystal mass.
Brief description of the drawings
Fig. 1 is the dual temperature area method crystal growing apparatus structural representation of the present invention.
Embodiment
The invention will be further described with reference to embodiments：
Dual temperature area method crystal growing apparatus of the present invention is integral type structure, and material uses but is not limited to quartz or glass material.
Temperature programmed control is carried out to upper and lower warm area to use but be not limited to resistance heating or lamp mode of heating.
Embodiment 1：Dual temperature area method crystal growing apparatus top is low-temperature space, has cup-shaped sandwich.Wherein, inner-layer cup
Internal diameter 85 mm, high 170 mm, the mm of wall thickness 5 of body 1；Internal diameter 200 mm, high 150 mm, the mm of wall thickness 5 of outer layer cup 2, bottom
For high-temperature region, in ball bottle-shaped, the mL of volume 25, for holding excessive solute and forming high temperature saturated solution；Pass through between upper and lower warm area
Straight tube 4 connects, the mm of straight tube internal diameter 10, long 100 mm, the mm of wall thickness 5, and is furnished with thermal baffle 5, the mm of thermal baffle diameter 140,
The mm of thickness 5, baffle plate bottom center is apart from the mm of 3 opening of pin 20, for heat-insulated and support heat-preservation cotton layer.Dual temperature area method crystal
Grower is integral type structure, using glass material.Dual temperature area method crystal growing apparatus top low-temperature space uses lamp heating side
Formula, bottom high-temperature region use resistance heating manner.
When dual temperature area method crystal growing apparatus is used to grow DAST crystal, into interlayer, water filling is as heating water bath inner-layer cup
Solution in body 1,5 g DAST sources powder, the DAST- that inner layer cup 1 is injected at 64 DEG C are added into bottom high-temperature region pin 3
After the mL of methanol saturated solution 450, interior outer cup is sealed by top blind flange；Temperature programmed control is carried out to upper and lower warm area respectively, if
The top low-temperature space bath temperature after temperature stabilization is determined for 30 DEG C and constant temperature, and top low-temperature space reaches set by slow cooling
Fixed temperature, 2.00 DEG C/d of rate of temperature fall, bottom high-temperature region temperature range are 67 DEG C and constant temperature.When top, low-temperature space temperature is
At 31 DEG C, size 2mm × 2mm × 0.1mm DAST seed crystals are put into by seed rod, by 15d growth, obtain one
Size 4.8mm × 4.3mm × 0.8mm DAST crystal.
Embodiment 2：Dual temperature area method crystal growing apparatus top is low-temperature space, has cup-shaped sandwich.Wherein, inner-layer cup
Internal diameter 90 mm, high 180 mm, the mm of wall thickness 10 of body 1；Internal diameter 180 mm, high 140 mm, the mm of wall thickness 10 of outer layer cup 2；Under
Portion is high-temperature region, in ball bottle-shaped, the mL of volume 50, for holding excessive solute and forming high temperature saturated solution；Lead between upper and lower warm area
Cross straight tube 4 to connect, the mm of straight tube internal diameter 20, long 150 mm, the mm of wall thickness 10, and be furnished with thermal baffle 5, thermal baffle diameter 130
Mm, the mm of thickness 10, baffle plate bottom center is apart from the mm of 3 opening of pin 20, for heat-insulated and support heat-preservation cotton layer.Dual temperature area method
Crystal growing apparatus is integral type structure, using quartz material.Dual temperature area method crystal growing apparatus top low-temperature space uses resistance
Mode of heating, bottom high-temperature region use lamp mode of heating.
When dual temperature area method crystal growing apparatus is used to grow DAST crystal, into interlayer, water filling is as heating water bath inner-layer cup
Solution in body 1,10 g DAST sources powder are added into bottom high-temperature region pin 3, and inner layer cup 1 is injected at 55 DEG C
After the mL of DAST- methanol saturated solution 850, interior outer cup is sealed by top blind flange；Line program control is entered to upper and lower warm area respectively
Temperature, the top low-temperature space bath temperature after design temperature is stable is 39 DEG C and constant temperature, and top low-temperature space is reached by slow cooling
Set temperature, 0.05 DEG C/d of rate of temperature fall, bottom high-temperature region temperature range are 56 DEG C and constant temperature.When top low-temperature space temperature
Spend for 40 DEG C when, size 2mm × 2mm × 0.1mm DAST seed crystals are put into by seed rod, by 20d growth, are obtained
One size 10mm × 9.5mm × 3mm DAST crystal.
Embodiment 3：Dual temperature area method crystal growing apparatus top is low-temperature space, has cup-shaped sandwich.Wherein, inner-layer cup
Internal diameter 87 mm, high 175 mm, the mm of wall thickness 6 of body 1；Internal diameter 190 mm, high 145 mm, the mm of wall thickness 6 of outer layer cup 2；Bottom
For high-temperature region, in ball bottle-shaped, the mL of volume 25, for holding excessive solute and forming high temperature saturated solution；Pass through between upper and lower warm area
Straight tube 4 connects, the mm of straight tube internal diameter 15, long 140 mm, the mm of wall thickness 6, and is furnished with thermal baffle 5, the mm of thermal baffle diameter 135,
Thickness 6mm, baffle plate bottom center is apart from the mm of 3 opening of pin 20, for heat-insulated and support heat-preservation cotton layer.Dual temperature area method crystal
Grower is integral type structure, using quartz material.Dual temperature area method crystal growing apparatus top low-temperature space uses lamp heating side
Formula, bottom high-temperature region use resistance heating manner.
When dual temperature area method crystal growing apparatus is used to grow DAST crystal, into interlayer, water filling is as heating water bath inner-layer cup
Solution in body 1,5 g DAST sources powder, the DAST- that inner layer cup 1 is injected at 60 DEG C are added into bottom high-temperature region pin 3
After the mL of methanol saturated solution 650, interior outer cup is sealed by top blind flange；Temperature programmed control is carried out to upper and lower warm area respectively, if
The top low-temperature space bath temperature after temperature stabilization is determined for 34 DEG C and constant temperature, and top low-temperature space reaches set by slow cooling
Fixed temperature, 1.00 DEG C/d of rate of temperature fall, bottom high-temperature region temperature range are 61 DEG C and constant temperature.When top, low-temperature space temperature is
At 35 DEG C, size 3mm × 3mm × 0.1mm DAST seed crystals are put into by seed rod, by 17d growth, obtain one
Size 5.5mm × 5.0mm × 1mm DAST crystal.
Embodiment 4：Dual temperature area method crystal growing apparatus top is low-temperature space, has cup-shaped sandwich.Wherein, inner-layer cup
Internal diameter 87 mm, high 175 mm, the mm of wall thickness 6 of body 1；Internal diameter 190 mm, high 145 mm, the mm of wall thickness 6 of outer layer cup 2；Bottom
For high-temperature region, in ball bottle-shaped, the mL of volume 25, for holding excessive solute and forming high temperature saturated solution；Pass through between upper and lower warm area
Straight tube 4 connects, the mm of straight tube internal diameter 15, long 140 mm, the mm of wall thickness 6, and is furnished with thermal baffle 5, the mm of thermal baffle diameter 135,
Thickness 6mm, baffle plate bottom center is apart from the mm of 3 opening of pin 20, for heat-insulated and support heat-preservation cotton layer.Dual temperature area method crystal
Grower is integral type structure, using quartz material.Dual temperature area method crystal growing apparatus top low-temperature space uses lamp heating side
Formula, bottom high-temperature region use resistance heating manner.
When dual temperature area method crystal growing apparatus is used to grow DAST crystal, into interlayer, water filling is as heating water bath inner-layer cup
Solution in body 1,8 g DAST sources powder, the DAST- that inner layer cup 1 is injected at 55 DEG C are added into bottom high-temperature region pin 3
After the mL of methanol saturated solution 850, interior outer cup is sealed by top blind flange；Temperature programmed control is carried out to upper and lower warm area respectively, if
The top low-temperature space bath temperature after temperature stabilization is determined for 39 DEG C and constant temperature, and top low-temperature space reaches set by slow cooling
Fixed temperature, 0.10 DEG C/d of rate of temperature fall, bottom high-temperature region temperature range are 56 DEG C and constant temperature.When top, low-temperature space temperature is
At 40 DEG C, size 3mm × 3mm × 0.1mm DAST seed crystals are put into by seed rod, by 64d growth, obtain one
Size 15mm × 13mm × 5mm DAST crystal.
In above-mentioned all embodiments, DAST crystal mass that embodiment 3 and embodiment 4 are obtained is more excellent, transmitance more
Height, therefore embodiment 3 and embodiment 4 are the preferred embodiments of the present invention, and using its technological parameter section as the excellent of the present invention
Select process program.
Claims (5)
- A kind of 1. dual temperature area method crystal growing apparatus, it is characterised in that：Dual temperature area method crystal growing apparatus top is low-temperature space, tool There is cup-shaped sandwich；Wherein, internal layer cup（1）Internal diameter be 85 ~ 90 mm, a height of 170 ~ 180 mm, wall thickness is 5 ~ 10 mm； Outer layer cup（2）Internal diameter be 180 ~ 200 mm, be high 140 ~ 150 mm, wall thickness is 5 ~ 10 mm；Dual temperature area method crystal growth dress It is high-temperature region to put bottom, and in ball bottle-shaped, volume is 25 mL or 50 mL, molten for holding excessive solute and forming high temperature saturation Liquid；Upper and lower low-temperature space and high temperature section pass through straight tube（4）Connection, straight tube internal diameter are 10 ~ 20 mm, a length of 100 ~ 150 mm, wall thickness For 5 ~ 10 mm, and it is furnished with thermal baffle（5）, a diameter of 130 ~ 140 mm of thermal baffle, thickness is 5 ~ 10 mm, thermal baffle （5）Bottom center is apart from pin（3）The mm of opening 20, for heat-insulated and support heat-preservation cotton layer.
- A kind of 2. dual temperature area method crystal growing apparatus according to claim 1, it is characterised in that：Dual temperature area method crystal growth Device is integral type structure, and material is using quartz or glass material.
- 3. one kind carries out DAST crystal growth techniques using dual temperature area method crystal growing apparatus as claimed in claim 1, it is special Sign is：When being used to grow DAST crystal using dual temperature area method crystal growing apparatus, into interlayer, water filling is as in heating water bath Layer cup（1）In solution, to bottom high-temperature region pin（3）Middle addition 5-10 g DAST sources powder, inner layer cup（1）Injection After DAST- methanol saturated solution 450-850 mL at 55-64 DEG C, interior outer cup is sealed by top blind flange；Respectively to upper Lower warm area carries out temperature programmed control, and the top low-temperature space bath temperature scope after design temperature is stable is 30-39 DEG C, bottom high temperature Area's temperature range is 56-67 DEG C；Top low-temperature space reaches set temperature, rate of temperature fall 0.05- by slow cooling 2.00 DEG C/d, it is set as temperature constant state after temperature stabilization；Bottom high-temperature region is set as temperature constant state all the time.
- 4. one kind according to claim 3 carries out DAST crystal growth techniques using dual temperature area method crystal growing apparatus, its It is characterised by：When dual temperature area method crystal growing apparatus is used to grow DAST crystal, into interlayer, water filling is as heating water bath internal layer Cup（1）In solution, to bottom high-temperature region pin（3）Middle addition 5-8 g DAST sources powder, inner layer cup（1）Inject 55- After DAST- methanol saturated solution 650-850 mL at 60 DEG C, interior outer cup is sealed by top blind flange；Respectively to upper and lower Warm area carries out temperature programmed control, and the top low-temperature space bath temperature scope after design temperature is stable is 34-39 DEG C, bottom high-temperature region Temperature range is 56-61 DEG C；Top low-temperature space reaches set temperature, rate of temperature fall 0.10-1.00 by slow cooling DEG C/d, it is set as temperature constant state after temperature stabilization；Bottom high-temperature region is set as temperature constant state all the time.
- 5. one kind according to claim 3 or claim 4 carries out DAST crystal using dual temperature area method crystal growing apparatus Growth technique, it is characterised in that：Temperature programmed control is carried out to upper and lower warm area and uses resistance heating or lamp mode of heating.
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