CN101440513A - Microscopic real-time visual crystal growth apparatus by solution method - Google Patents
Microscopic real-time visual crystal growth apparatus by solution method Download PDFInfo
- Publication number
- CN101440513A CN101440513A CNA2008102381996A CN200810238199A CN101440513A CN 101440513 A CN101440513 A CN 101440513A CN A2008102381996 A CNA2008102381996 A CN A2008102381996A CN 200810238199 A CN200810238199 A CN 200810238199A CN 101440513 A CN101440513 A CN 101440513A
- Authority
- CN
- China
- Prior art keywords
- solution
- crystal
- growth
- crystal growth
- real
- 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
Images
Abstract
The invention relates to a micrographic real-time direct viewing type solution method crystal growth device for micrographic real-time viewing and analysis in the solution method crystal growth process. A temperature control meter is arranged at the top of the device, connected with a thermocouple through electric information, and communicated with an infrared heating lamp through temperature transmission; an electric thermocouple and a circulating pump are vertically arranged in a growth solution in a solution jar made of transparent glass; the circulating pump passes through a solution duct and runs through a crystal growth groove to form a circulation loop; the periphery of the solution jar is provided with a transparent glass outer jar, wherein two side walls of the transparent glass outer jar are provided with the infrared heating lamp respectively, while the lower part is provided with a computer and a microscope objective lens; and a growing crystal is arranged in the crystal growth groove with a box structure. The device has the advantages of simple and novel structure, low manufacturing cost, flexible and convenient use and operation, real-time observation and reliable analysis principle.
Description
Technical field:
The present invention relates in a kind of crystal growth from solution process can micro-real-time direct viewing and the device systems of analysis, particularly a kind of microscopic real-time visual crystal growth apparatus by solution method that is applicable to the various water-soluble crystal of Real Time Observation, organic crystal growth surface pattern, be used to observe the microstructure and the shape characteristic of crystal growing surface, the lattice defect forming process of the growth mechanism of analyzing crystal and micro-scale.
Background technology:
The research of mechanism of crystal growth in more than 100 year time, has been experienced theoretical 3 stages of crystal equilibrium attitude theory, interface growth theory and PBC (periodical chain chain) in the past.The Zhong Weizhuo of Shanghai silicate institute has proposed negative ion coordination polyhedron growth unit theoretical model [Zhang Xuehua; Luo Hao Sue in early 1990s, Zhong Weizhuo. negative ion coordination polyhedron growth unit model and the application in crystal growth thereof. Chinese science, 2004,34 (3): 241-253.], these models have been made explanation to crystal growing process in some aspects, but shortcoming is separately all arranged, so these theories can't instruct the crystal growth practice well.It is research mechanism of crystal growth and the most effective means of crystal growth defective that crystal growing surface is carried out the real-time monitored analysis.Be subjected to the restriction of crystal growth temperature and condition, the high temperature crystal growth process is difficult to carry out the real-time monitored analysis, is model with the crystal growth of cryogenic fluid method substantially to the research of mechanism of crystal growth.Crystal growth real-time monitored means commonly used at present mainly contain laser phase-shifting interferometer, laser holographic interferometry and atomic force microscope etc.Laser holographic interferometry can study the solid-liquid boundary layer structure and the dynamic variation process of crystal growing surface [1, Yu Xiling, the method for real-time measuring crystal growth solid/liquid interfaces and boundary layer structure, 1998, the patent No. (CN 1190738); 2, Zhao Peng, Xia Hairui, Sun Daliang etc. utilize the influence of holographic phase contrast interference microscope research EDTA, artificial lens journal, 2003,32 (1): 31-34. to the KDP Growth Habit], but can't intuitively observe the pattern of crystal growing surface; The laser phase-shifting interferometer can the analyzing crystal surface information [Nicholas A.Booth such as growth hillock structure, .Differential phase-shifting interferometry in situ surfacecharacterization during solution growth of crystals.Review ofscientific instruments such as Boris Stanojev, 2002, the step appearance information that 73 (10): 3540-3545.], still also can't intuitively reflect growth surface; Atomic force microscope can differentiate detailed surface topography such as the single basic step of crystal growing surface and growth hillock etc. and constitutional features [1, Yang Shangfeng, .Surface topography of rapidly grownKH2PO4 crystals with additives:ex situ investigation by atomicforce microscopy.Journal of Crystal Growth such as Su Genbo, 1999,203:425-433.; 2, T.N.Thomas .AFM investigation of step kineticsand hillock morphology of the{100}face of KDP[J such as T.A.Land] .Journalof Crystal Growth, 2004,260:566-579.].But there are two important disadvantages in AFM: the scanning area of (1) AFM is very little, and the maximum scan zone of report is 100 * 100 μ m
2, and the length range that the step bundle develops is millimetre-sized.(2) AFM scanning obtains the time span order of magnitude of an image and is minute, and the order of magnitude of the step speed of growth is 1 μ s
-1Therefore AFM to the real-time study limitation of crystal growth kinetics in slow growth kinetics.And AFM costs an arm and a leg, to the requirement for experiment condition harshness, and the operation of equipment complexity.
Summary of the invention:
The objective of the invention is to overcome the shortcoming that exists in the prior art, seek to design the real-time monitored that provides a kind of novelty simple in structure, enforcement convenience, low cost of manufacture, maneuverable real-time monitored system and device to realize the crystal growth from solution process, the evolutionary process of analyse crystal growth surface macrosteps and defective forming process, research crystalline growth mechanism and physicals.To carry out Real Time Observation to crystal growing process, at first will satisfy crystal normal growth conditions needed: the one, accurate control growing solution temperature; The 2nd, growth solution flows at crystal growing surface; Utilize opticmicroscope that crystal growing surface is carried out microscopic observation simultaneously, need the small design crystal growing apparatus, and crystallizer there is transparent observation window.
To achieve these goals, the system and device that the present invention relates to is divided into temperature control, crystallizer, solution circulated is mobile and four integral parts of microscopic observation; Agent structure comprises temp controlled meter, thermopair, infrared heat lamp, water circulating pump, solution tank, outer shell, growth solution, hot plate, micro objective, crystal growth groove, growing crystal, solution conduit and computer; Agent structure is set to integrated device.
Temperature control part branch of the present invention comprises temp controlled meter, thermopair, infrared heat lamp and hot plate; Gather the temperature signal of growth solution and import temp controlled meter into thermopair, temp controlled meter is realized the automated intelligent control of growth solution by the heating power of control infrared heat lamp according to the experiment preset program.
Crystallizer part of the present invention is made up of crystal growth groove and growing crystal, can satisfy the needed primary condition of aqueous solution crystal growth, the saturated solution that circulates through temperature control can make crystal grow under desired degree of supersaturation, saturated solution makes plane of crystal growth solution degree of supersaturation even with certain flow velocity through crystal growing surface, and the growth groove is to be bonded with poly (methyl methacrylate) plate.
Solution circulated of the present invention flows and partly is made up of water circulating pump and solution conduit, and water circulating pump is connected with continuously variable transformer, comes the flow velocity of growth solution in the stepless control device by the output voltage of adjusting transformer.
Microscopic observation part of the present invention cooperates connection to constitute by microscope and computer, crystal growing process in the small-sized crystallizer can be directly by microscopic examination, utilize the IMAQ program in the computer, microprocess to crystal growth in the crystallizer carries out Real Time Observation, takes pictures and records a video, obtain picture and video data by analysis, also obtain the various dynamics datas in the crystal growing process and the evolutionary process of growth surface structure, and then the microprocess of crystal growth is carried out deep analysis.
When apparatus of the present invention realize, temp controlled meter is arranged on the device top and is connected with thermopair telecommunications breath, and be communicated with the transmission of Infrared Heating light temperature, 70%～80% the mid-growth solution of depositing in space in the solution tank that transparent glass is made, vertically be provided with electroheat pair in the growth solution, growth solution is provided with water circulating pump in the top, and water circulating pump forms circulation loop through solution conduit and the crystal growth groove of bottom of device of going here and there, and the end of the backhaul section of solution conduit is connected the bottom in solution tank; The solution tank periphery is shaped on the outer shell of transparent glass physique, on the wall of the outer shell left and right sides respectively symmetrical structure be shaped on infrared heat lamp, directly solution in the subtend solution tank and heating, symmetry is oblique between solution tank bottom surface and the outer shell bottom surface is provided with two hot plates, outer shell bottom surface bottom is provided with computer, the growing crystal in the direct subtend crystal growth of the micro objective groove is equipped with in the computer bottom, the information of its micro objective collection is directly imported computer, bottom of device is provided with the crystal growth groove of box structure, its inside is provided with growing crystal, and shower comes from the growth solution of solution conduit.
The present invention compared with prior art, its general arrangement novelty simple in structure, preparation cost is low, uses operation nimble, Real Time Observation and analysis principle are reliable, particularly can provide theory and field data intuitively for the many physicalies in postgraduate's long crystal process effectively.
Description of drawings:
Fig. 1 is a composition structural principle synoptic diagram of the present invention
Embodiment:
Also be described further in conjunction with the accompanying drawings below by embodiment.
Embodiment:
The system and device that present embodiment relates to is divided into temperature control, crystallizer, solution circulated is mobile and four integral parts of microscopic observation; Agent structure comprises temp controlled meter, thermopair, infrared heat lamp, water circulating pump, solution tank, outer shell, growth solution, hot plate, micro objective, crystal growth groove, growing crystal, solution conduit and computer; Agent structure is set to integrated device.When apparatus of the present invention realize, temp controlled meter is arranged on the device top and is connected with thermopair telecommunications breath, and be communicated with the transmission of Infrared Heating light temperature, 70%～80% the mid-growth solution of depositing in space in the solution tank that transparent glass is made, vertically be provided with electroheat pair in the growth solution, growth solution is provided with water circulating pump in the top, and water circulating pump forms circulation loop through solution conduit and the crystal growth groove of bottom of device of going here and there, and the end of the backhaul section of solution conduit is connected the bottom in solution tank; The solution tank periphery is shaped on the outer shell of transparent glass physique, on the wall of the outer shell left and right sides respectively symmetrical structure be shaped on infrared heat lamp, directly solution in the subtend solution tank and heating, symmetry is oblique between solution tank bottom surface and the outer shell bottom surface is provided with two hot plates, outer shell bottom surface bottom is provided with computer, the growing crystal in the direct subtend crystal growth of the micro objective groove is equipped with in the computer bottom, the information of its micro objective collection is directly imported computer, bottom of device is provided with the crystal growth groove of box structure, its inside is provided with growing crystal, and shower comes from the growth solution of solution conduit.
The use of present embodiment, the growing crystal 11 that at first will observe is fixed on sealing in the crystal growth groove 10, the growth crystal face of observing is parallel to view port, connect the power supply of water circulating pump 4, the growth solution 7 of the Overheating Treatment after filtration in the solution tank 5 is circulated in system, crystal in the crystal growth groove 10 begins growth, the real-time information that utilizes microscope 9 and computer 13 to gather crystal growing surface, analyse crystal growth process; Come the flow velocity of regulator solution by the voltage of regulating water circulating pump 4, utilize FP93 temp controlled meter 1 to come the degree of supersaturation of control growing solution 7; Can in test process, introduce impurity in addition and compare experiment.
Claims (5)
1, a kind of microscopic real-time visual crystal growth apparatus by solution method is divided into temperature control, crystallizer, solution circulated and flows and four integral parts of microscopic observation; Agent structure comprises temp controlled meter, thermopair, infrared heat lamp, water circulating pump, solution tank, outer shell, growth solution, hot plate, micro objective, crystal growth groove, growing crystal, solution conduit and computer; Agent structure is set to integrated device, it is characterized in that temp controlled meter is arranged on the device top and is connected with thermopair telecommunications breath, and be communicated with the transmission of Infrared Heating light temperature, 70%～80% the mid-growth solution of depositing in space in the solution tank that transparent glass is made, vertically be provided with electroheat pair in the growth solution, growth solution is provided with water circulating pump in the top, water circulating pump forms circulation loop through solution conduit and the crystal growth groove of bottom of device of going here and there, and the end of the backhaul section of solution conduit is connected the bottom in solution tank; The solution tank periphery is shaped on the outer shell of transparent glass physique, on the wall of the outer shell left and right sides respectively symmetrical structure be shaped on infrared heat lamp, directly solution in the subtend solution tank and heating, symmetry is oblique between solution tank bottom surface and the outer shell bottom surface is provided with two hot plates, outer shell bottom surface bottom is provided with computer, the growing crystal in the direct subtend crystal growth of the micro objective groove is equipped with in the computer bottom, the information of its micro objective collection is directly imported computer, bottom of device is provided with the crystal growth groove of box structure, its inside is provided with growing crystal, and shower comes from the growth solution of solution conduit.
2, microscopic real-time visual crystal growth apparatus by solution method according to claim 1 is characterized in that the temperature control part branch comprises temp controlled meter, thermopair, infrared heat lamp and hot plate; Gather the temperature signal of growth solution and import temp controlled meter into thermopair, temp controlled meter is realized the automated intelligent control of growth solution by the heating power of control infrared heat lamp according to the experiment preset program.
3, microscopic real-time visual crystal growth apparatus by solution method according to claim 1, it is characterized in that crystallizer part is made up of crystal growth groove and growing crystal, the saturated solution that circulates through temperature control is grown crystal under degree of supersaturation, saturated solution makes plane of crystal growth solution degree of supersaturation even through crystal growing surface.
4, microscopic real-time visual crystal growth apparatus by solution method according to claim 1, it is characterized in that the solution circulated part that flows is made up of water circulating pump and solution conduit, water circulating pump is connected with continuously variable transformer, comes the flow velocity of growth solution in the stepless control device by the output voltage of adjusting transformer.
5, microscopic real-time visual crystal growth apparatus by solution method according to claim 1, it is characterized in that the microscopic observation part cooperates connection to constitute by microscope and computer, crystal growing process is directly by microscopic examination, utilize the IMAQ program in the computer, microprocess to crystal growth carries out Real Time Observation, takes pictures and records a video, obtain picture and video data by analysis, also obtain the various dynamics datas in the crystal growing process and the evolution of growth surface structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102381996A CN101440513A (en) | 2008-12-05 | 2008-12-05 | Microscopic real-time visual crystal growth apparatus by solution method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102381996A CN101440513A (en) | 2008-12-05 | 2008-12-05 | Microscopic real-time visual crystal growth apparatus by solution method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101440513A true CN101440513A (en) | 2009-05-27 |
Family
ID=40725112
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008102381996A Pending CN101440513A (en) | 2008-12-05 | 2008-12-05 | Microscopic real-time visual crystal growth apparatus by solution method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101440513A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177713A (en) * | 2015-08-07 | 2015-12-23 | 青岛大学 | Organic pyridinium salt crystal growth control method |
| CN108165486A (en) * | 2017-12-27 | 2018-06-15 | 大连理工大学 | A kind of experimental system and method suitable for macromolecule crystallization process accuracy controlling |
| WO2019128766A1 (en) * | 2017-12-27 | 2019-07-04 | 大连理工大学 | Experimental system and method applicable to precise regulation of macromolecular crystallization processes |
-
2008
- 2008-12-05 CN CNA2008102381996A patent/CN101440513A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177713A (en) * | 2015-08-07 | 2015-12-23 | 青岛大学 | Organic pyridinium salt crystal growth control method |
| CN105177713B (en) * | 2015-08-07 | 2018-05-08 | 青岛大学 | A kind of organic pyridinium salt crystal growth control method |
| CN108165486A (en) * | 2017-12-27 | 2018-06-15 | 大连理工大学 | A kind of experimental system and method suitable for macromolecule crystallization process accuracy controlling |
| WO2019128766A1 (en) * | 2017-12-27 | 2019-07-04 | 大连理工大学 | Experimental system and method applicable to precise regulation of macromolecular crystallization processes |
| CN108165486B (en) * | 2017-12-27 | 2021-04-20 | 大连理工大学 | Experimental system and method suitable for precise regulation and control of macromolecule crystallization process |
| US11452948B2 (en) | 2017-12-27 | 2022-09-27 | Dalian University Of Technology | Experiment system and method for accurate controlling of macromolecular crystallization process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11650406B2 (en) | Microscopic imaging method of phase contrast and differential interference contrast based on the transport of intensity equation | |
| CN103091181B (en) | Miniature stretching rheological device for in-situ structure detection of polymer film material, and experimental method thereof | |
| CN100590437C (en) | Total reflection near-field microscope combining with magnetic forceps for observing biomacromolecule | |
| CN101440513A (en) | Microscopic real-time visual crystal growth apparatus by solution method | |
| CN111239132B (en) | Visual high-pressure microfluidic hydrate simulation experiment device and application thereof | |
| CN103603029A (en) | Crystal preparation apparatus with transparent structure | |
| CN108572189A (en) | The force model comprehensive test system of soil body harmomegathus characteristic under a kind of consideration temperature gradient | |
| CN201305644Y (en) | Micrographic real-time direct viewing type solution method crystal growing apparatus | |
| Wu et al. | Measurement of crystal face specific growth kinetics | |
| CN102183397B (en) | Fully-automatic closed type tissue dehydrator | |
| JP2005306827A (en) | Method and device for rapid purification/measurement of biopolymer crystal | |
| CN110231228A (en) | Thickness is to the plate corrugation performance test apparatus and application method under stress | |
| CN106018467A (en) | Visual large vessel boiling experiment device | |
| CN206710343U (en) | One kind scanning low-angle scattering of X-rays micro-fluidic detection experimental provision | |
| CN103344565A (en) | Temperature-controlled magnetic tweezer device | |
| CN103941437B (en) | Experimental facility used for high-low temperature optical evaluation | |
| CN208860634U (en) | A kind of visualized operation oscillatory type deposit collection monitoring system | |
| CN208351147U (en) | A kind of medical imaging observation ancillary equipment | |
| CN201413339Y (en) | Single-camera Doppler global velocity measuring device | |
| Zhang et al. | Comprehensive numerical simulation analysis of flow and mass transfer by tuning inlet conditions in solution circulating technique focused to grow quality KDP crystal | |
| WO2021073245A1 (en) | Single-frame differential phase contrast quantitative phase imaging method based on color multiplexing illumination | |
| CN204536154U (en) | A kind ofly collecting and distributingly to penetrate, the micro-stream in one becomes original position Online Transaction Processing | |
| JP4117341B2 (en) | Hot water circulation microscope culture chamber | |
| CN207947758U (en) | A kind of signal generator easy to operation and with defencive function of flexible structure | |
| CN207866196U (en) | A kind of diaphragm detection device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20090527 |