CN1032369A - The method and apparatus of using rotary disk method to grow pure sulphuric-acid tripeptide glycol crystal - Google Patents

The method and apparatus of using rotary disk method to grow pure sulphuric-acid tripeptide glycol crystal Download PDF

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Publication number
CN1032369A
CN1032369A CN 88103965 CN88103965A CN1032369A CN 1032369 A CN1032369 A CN 1032369A CN 88103965 CN88103965 CN 88103965 CN 88103965 A CN88103965 A CN 88103965A CN 1032369 A CN1032369 A CN 1032369A
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crystal
seed crystal
rotating disk
solution
educating
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缪明明
杨宗璐
阮进科
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Yunnan University YNU
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Yunnan University YNU
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B7/00Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

A kind of method and apparatus of using rotary disk method to grow pure sulphuric-acid tripeptide glycol crystal belongs to infrared thermal release electric detector and infrared thermal imaging technique field.
The present invention overcomes deficiency of the prior art, adopts using rotary disk method to grow pure sulphuric-acid tripeptide glycol crystal.The sulfuric acid 3-gsh crystal of the present invention growth has transparent and homogeneous, and performance is good, and internal stress is little, very easily cuts exactly by cleavage surface during section, and growth cycle is short, and material use efficiency is up to 80% with first-class advantage, also can be by need the grow crystal of different size of user.

Description

The method and apparatus of using rotary disk method to grow pure sulphuric-acid tripeptide glycol crystal
The present invention relates to a kind of rotating disk method growth bright sulfur acid triglycine crystalline method and apparatus, belong to infrared thermal release electric detector and infrared thermal imaging technique field.
Up to now, domestic and international plain sulfuric acid 3-gsh crystal all adopts shaft-like seeded growth, when this method is made the big area target surface to crystal cut, exist the crystal cleavage surface to be difficult to make an accurate selection of and material use efficiency low (<40%), problems such as growth cycle is long, England Impco electrical engineering department in 1975 has at first been released the rotating disk method and has been come oriented growth doped sulfuric acid triglycine crystal, basically overcome the uneven shortcoming of mixing, but increase with internal stress in the crystal of this method growth, crystal breaks in the making processes of device easily, has increased the difficulty of manufacture craft.
International online retrieval world patent, CA, Britain's science abstract are not seen with rotating disk method growth bright sulfur acid triglycine crystalline bibliographical information.
The objective of the invention is to overcome above-mentioned weak point of the prior art and a kind of rotating disk method growth bright sulfur acid triglycine crystalline method and apparatus is provided.
Purpose of the present invention can reach by following measure: hexagonal plane seed crystal adopts wet line patterning method that the cleavage surface of sheet seed crystal along triglycine sulfate cut down, on the fine sandpaper of band water, grinding, make its surfacing, smooth, the seed crystal after the polishing is put into by educating the growing apparatus that brilliant device, tank and Controlling System are formed behind cleaning, airing.Educating brilliant device is loaded on and is provided with stirring arm, in the tank of heating unit and sensor, stirring arm in the tank rotatablely moves in the same way, the temperature controlling system that water temperature is made up of temperature sensitization apparatus and thermistor temperature controller is controlled between 20 °~70 ℃, the rotating speed of educating rotating disk in the brilliant device is controlled at per minute 20~40 to be changeed, and the contact surface of rotating disk and sexangle plane seed crystal is shape plane, garden.Educating the saturation point of growth mother liquid in the brilliant device measures through bigness scale, thin survey, accurate measurement three processes, its three process is respectively: bigness scale ties up to and drops into one little sulfuric acid 3-gsh crystal in the solution, observe its variation of shape size in solution, when the shape size of sulfuric acid 3-gsh crystal stopped to change, the temperature of looking this moment was the bigness scale saturation point; The thin survey ties up on the rotating disk sticking synthetic glass crystalline style of pulling, and in this root crystalline style end of pulling, fixes a shaft-like seed crystal with sebific duct, observe the concentration eddy current of shaft-like seed crystal, the regulator solution temperature disappears until eddy current, and the temperature when looking the eddy current disappearance is that solution is carefully surveyed saturation point; Accurate measurement system is bonded at a sheet triglycine sulfate seed crystal on the rotating disk as exploratory seed crystal, place in the solution, garden dish rotating speed is 20~40 rev/mins, through 20~24 hours constant temperature, observes seed crystal face, when crystal face smooth, when corner angle were clearly demarcated, this temperature was exactly the accurate measurement temperature of saturation of solution, promptly was the saturation point of bright sulfur acid triglycine crystal growth, this moment, the pH value with its solution was controlled between 1.85~1.95, grew pure sulfuric acid 3-gsh crystal under these conditions.
Purpose of the present invention can also reach by following measure: be provided with one by three isometric glass supporter fixed shelves stream glass garden tubes in educating brilliant device, for making solute arrive crystal growing surface equably through the garden tube heat build-up of shelves stream glass, shelves are flowed the top of glass infuser and the distance of rotating disk face is controlled at 2~3Cm, be the thermograde in the minimizing solution and the volatilization of solution, educate the sealing cover of brilliant device and be made up of the rubber of two blocks of close bakelites and a 4mm, rubber is placed between two blocks of bakelites.
Accompanying drawing is a bright sulfur acid triglycine growing method process flow sheet.
The present invention is described in further detail below in conjunction with (accompanying drawing) embodiment: sexangle plane seed crystal adopts wet line patterning method that the cleavage surface of sheet seed crystal along sulfuric acid 3-gsh crystal cut down, its thickness is 2~2.5mm, the blank seed crystal is ground on the fine sandpaper of band water, seed crystal after its surfacing, smooth, the polishing is bonded at after cleaning, drying on the dish of garden, is positioned over by educating in the growing apparatus that brilliant device, tank and Controlling System form.Educating brilliant device is loaded on and is provided with stirring arm, in the tank of heating unit and temperature sensitization apparatus, stirring arm in the tank rotatablely moves in the same way, the stirring arm rotating speed is that per minute 100 changes, the temperature controlling system that water temperature is made up of temperature sensitization apparatus and thermistor temperature controller is controlled between 20 ℃~70 ℃, the growth mother liquid of educating in the brilliant device is preparation like this: at first glycine and 1: 1 sulfuric acid of volume were dropped into reaction cylinder (reaction cylinder has agitator and temperature regulating device) in 3: 1 in molar ratio, be chilled to 10 ℃ of crystallizations in reaction under 60 ℃ after tens hours, take out sulfuric acid 3-gsh crystal, with sulfuric acid 3-gsh crystal crystallization twice in redistilled water, dry stand-by again.To be mixed with mother liquor by certain saturation ratio through the sulfuric acid 3-gsh crystal of pure system then.The saturation point of growth mother liquid is measured through bigness scale, thin survey, accurate measurement three processes, its three process is respectively: bigness scale ties up to and drops into one little sulfuric acid 3-gsh crystal in the solution, observing the variation of its shape size in solution (is the crystal face " scared " of sulfuric acid 3-gsh crystal, faceted pebble occurs, some small-particle sundry goods or corner angle garden dish appear in cylinder bottom, volume reduces), through the regulator solution temperature, the shape of sulfuric acid 3-gsh crystal stops to change in solution, and the temperature of looking this moment is the bigness scale saturation point; The thin survey ties up on the rotating disk sticking synthetic glass crystalline style of pulling, fuse with will pull crystalline style and shaft-like seed crystal of sebific duct, place in the mother liquor, rotating speed is 20~40 rev/mins, observe the concentration eddy current of shaft-like seed crystal, the regulator solution temperature disappears until eddy current, and looking eddy current disappearance temperature is that solution is carefully surveyed saturation point; Accurate measurement system is bonded at a sheet triglycine sulfate seed crystal on the rotating disk as souning out seed crystal, place in the solution, rotating speed is 20~40 rev/mins, through 20~24 hours constant temperature, observe the surface of seed crystal, if crystal face is smooth, corner angle are clearly demarcated, this temperature is exactly the accurate measurement temperature of saturation of solution, promptly is bright sulfur acid triglycine crystal growth saturation point.This moment, the pH value with its solution was controlled between 1.85~1.95, grew pure sulfuric acid 3-gsh crystal under these conditions.
Being used to grow is provided with one in the brilliant device of educating of sulfuric acid 3-gsh crystal by three isometric glass supporter fixed shelves stream glass garden tubes, arrives crystal growing surface equably for making the solute through the garden tube heat build-up of shelves stream glass.The top of shelves stream glass garden tube and the distance of rotating disk face are controlled at 2~3Cm.For the thermograde in the minimizing solution and the volatilization of solution, to educate brilliant device sealing cover and form by the rubber of two blocks of bakelites and a 4mm, rubber is placed between two blocks of bakelites.
The contriver grows the pure sulfuric acid 3-gsh crystal that 4 sizes do not wait with above-mentioned method and apparatus.
The present invention has following advantage compared to existing technology:
1, pure sulfuric acid 3-gsh crystal has transparent and homogeneous, and performance is good, and internal stress is little, very easily cuts exactly by cleavage surface during section, and growth cycle is short, and stock utilization is up to more than 80%.
2, can grow according to user's needs the crystal of different size.

Claims (6)

1, a kind of rotating disk method growth bright sulfur acid triglycine crystalline method, seed crystal is put into by educating the growing apparatus that brilliant device, tank and Controlling System are formed, growing crystal under certain condition, it is characterized in that educating the saturation point of growth mother liquid in the brilliant device through bigness scale, thin survey, accurate measurement three processes mensuration, pH value is controlled between 1.85~1.95, its rotating speed of rotating disk of educating in the brilliant device is controlled at per minute 20~40 commentaries on classics, and its seed crystal is made into sexangle plane seed crystal.
2, by the said method of claim 1, the making system that it is characterized in that sexangle plane seed crystal adopts wet line patterning method that the cleavage surface of sheet seed crystal by sulfuric acid 3-gsh crystal cut down, on the fine sandpaper of band water, grind, make seed crystal after its surfacing, smooth, the polishing through cleaning, being bonded on the dish of garden and can using behind the airing.
3, by the said method of claim 1, it is characterized in that bigness scale, thin survey, accurate measurement three processes that the growth mother liquid saturation point is measured are respectively: bigness scale ties up to and drops into one little sulfuric acid 3-gsh crystal in the solution, observe its variation of shape size in solution, when the shape size of sulfuric acid 3-gsh crystal stopped to change, the temperature of looking this moment was the saturation point of bigness scale; The thin survey ties up on the rotating disk sticking synthetic glass crystalline style of pulling, and in this root crystalline style end of pulling, fixes a shaft-like seed crystal with sebific duct, observe the concentration eddy current of shaft-like seed crystal, the regulator solution temperature disappears until eddy current, and the temperature when looking the eddy current disappearance is that solution is carefully surveyed saturation point; Accurate measurement system is bonded at a sheet triglycine sulfate seed crystal on the rotating disk as exploratory seed crystal, place in the solution, the rotating disk rotating speed is controlled at 20~40 rev/mins, through 20~24 hours constant temperature, observe the surface of seed crystal, when crystal face smooth, when corner angle are clearly demarcated, this temperature is exactly the refining temperature of saturation of solution, promptly is the saturation point of bright sulfur acid triglycine crystal growth.
4, a kind of rotating disk method growth bright sulfur acid triglycine crystalline equipment that is used for, it is characterized in that educating and be provided with one in the brilliant device by three isometric glass supporter fixed shelves stream glass garden tubes, for making the solute through the garden tube heat build-up of shelves stream glass arrive crystal growing surface equably, the top of shelves stream glass garden tube and the distance of rotating disk face are controlled at 2~3Cm.
5, by the said equipment of claim 4, it is characterized in that the sealing cover of educating brilliant device is made up of the rubber of two blocks of bakelites and a 4mm, rubber is placed in the middle of two blocks of bakelites, and this structure can reduce the volatilization of the thermograde in the solution.
6, by claim 4,5 said equipment, it is characterized in that educating the rotating disk in the brilliant device and the contact surface of sexangle plane seed crystal is shape plane, garden.
CN 88103965 1988-06-23 1988-06-23 The method and apparatus of using rotary disk method to grow pure sulphuric-acid tripeptide glycol crystal Pending CN1032369A (en)

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CN 88103965 CN1032369A (en) 1988-06-23 1988-06-23 The method and apparatus of using rotary disk method to grow pure sulphuric-acid tripeptide glycol crystal

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Application Number Priority Date Filing Date Title
CN 88103965 CN1032369A (en) 1988-06-23 1988-06-23 The method and apparatus of using rotary disk method to grow pure sulphuric-acid tripeptide glycol crystal

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115233285A (en) * 2022-07-20 2022-10-25 江西新余新材料科技研究院 Crystal growth apparatus and method, and TGS-based crystal

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115233285A (en) * 2022-07-20 2022-10-25 江西新余新材料科技研究院 Crystal growth apparatus and method, and TGS-based crystal
CN115233285B (en) * 2022-07-20 2024-03-15 江西新余新材料科技研究院 Crystal growth device and method and TGS crystal

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