CN105568360A - Device and method for compounding zinc oxide single crystal material through hydrothermal method - Google Patents
Device and method for compounding zinc oxide single crystal material through hydrothermal method Download PDFInfo
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- CN105568360A CN105568360A CN201610137960.1A CN201610137960A CN105568360A CN 105568360 A CN105568360 A CN 105568360A CN 201610137960 A CN201610137960 A CN 201610137960A CN 105568360 A CN105568360 A CN 105568360A
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- 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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- 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
- C30B29/16—Oxides
Abstract
The invention relates to a device and a method for compounding a zinc oxide single crystal material through a hydrothermal method, which are capable of solving the problems that during a process of compounding single crystals by using the hydrothermal method, regulation of system factors is difficult and massive-block single crystals cannot be compounded. A technical scheme adopted by the invention is that the device comprises a regulating tank, a communicating pipe and a reaction tank, wherein an inner cavity of the regulating tank is communicated with an inner cavity of the reaction tank through the communicating pipe; the regulating tank and the reaction tank are of the same structure, namely, the regulating tank and the reaction tank are both of closed hollow structures; tank body liners which are made of heat-resisting and chemical corrosion-resisting materials are arranged in the inner cavities of the regulating tank and the reaction tank; a pipe body liner which is made of a heat-resisting and chemical corrosion-resisting material is arranged at the inner side of the communicating pipe. The method disclosed by the invention is novel, unique, simple and reasonable, has a function of compounding multiple inorganic crystals and has an important significance to scientific research and medicament; the device disclosed by the invention has the advantages of simpleness, easiness in operation and good effect, and is a technological innovation on hydrothermal preparation of crystals.
Description
Technical field
The present invention relates to hydrothermal method Zinc oxide single crystal materials synthesis device and synthetic method.
Background technology
Synthetic zincite crystal material passes through complicated physical and chemical reaction by compound crystal out under certain temperature and pressure, forms the process of monocrystalline or regular polycrystalline.Single-crystal zinc-oxide has decisive role for the development of the industries such as microelectronics, unicircuit, photovoltaic, laser equipment.Building-up process needs the factor such as temperature, pressure, concentration, composition transfer process of the accurate hierarchy of control.In the water heat transfer technology of current use, mainly concentrating on the technology such as temperature, pH value controlled in homogeneous liquid phase makes crystal separate out, due to hydrothermal method confined reaction under comparatively high temps and larger pressure usually, be difficult to realize so the reaction conditions in homogeneous liquid phase changes, and this method is suitable only for the monocrystalline preparing micro-or nano size, be difficult to synthesis large size single crystal.When China's laser equipment, micro-electronic device are growing to large size single crystal demand, this synthetic method cannot adapt to the development of contemporary scientific technology, extremely urgent to the technical renovation of composite crystals aspect.
Summary of the invention
For above-mentioned situation, for overcoming the defect of prior art, the object of the present invention is just to provide a kind of hydrothermal method Zinc oxide single crystal materials synthesis device and synthetic method, can effectively in solution water heat transfer monocrystalline process system factor regulate difficulty, the problem of agglomerate body monocrystalline cannot be synthesized.
The technical scheme that the present invention solves is, a kind of hydrothermal method Zinc oxide single crystal materials synthesis device, comprise regulating tank 1, communicating pipe 2 and retort 3, the inner chamber of regulating tank is through the intracavity inter-connection of communicating pipe and retort, regulating tank 1 is identical with the structure of retort 3, be airtight hollow structure, the inner chamber of the two all arranges the tank body liner 6 be made up of heat-resisting chemical resistant material, and the inner side of communicating pipe 2 is provided with the body liner 13 be made up of heat-resisting chemical resistant material.
Comprise the first body 2a be connected with regulating tank described communicating pipe 2, the the second body 2b be connected with retort 3 and be connected the first body, the adapter sleeve 21 of the second body, one end outer wall that first body is connected with the second body is provided with silk braid plug 16, on the first body and the second body, the silk braid 17 slided along respective body is provided with inside silk braid plug 16, silk braid outer wall there is the first outside screw 18, the inwall of adapter sleeve there is first internal thread 22 corresponding with the first outside screw, first body and the second body are by the first outside screw, first internal thread is together with pipe connecting spinning, flow control pad 23 has been clamped between inherent first body of adapter sleeve and the end face of the second body, there is ventilating pit 14 at flow control pad 23 center.
Described regulating tank 1 is identical with the structure of retort 3, include the shell 5 that explosion-proof metallic substance is made, tank body liner 6 and lid cover 4, shell and liner are the hollow structure of upper opening, neck bush is cased, liner upper end outer wall is provided with the seal convexity 15 compressing edge on housing mouth, lid cover 4 is the hollow structure of upper and lower opening, lid cover 4 inwall is provided with the second internal thread 9, outer shell outer wall is provided with second outside screw 10 corresponding with the second internal thread, lid cover is contained in shell upper by the second internal thread and the second external thread rotary, one end that first body is connected with regulating tank, one end that second body is connected with retort is provided with the sealing cover 11 of outwardly convex, under sealing cover is placed in lid cover and between seal convexity, be connected and sealed by screwing lid cover, integrant sealed structure.
A kind of hydrothermal method Zinc oxide single crystal material synthesis method, comprises the following steps:
A, installation synthesizer
Synthesizer comprises regulating tank 1, communicating pipe 2 and retort 3, the inner chamber of regulating tank is through the intracavity inter-connection of communicating pipe and retort, regulating tank 1 is identical with the structure of retort 3, be airtight hollow structure, the inner chamber of the two all arranges the tank body liner 6 be made up of heat-resisting chemical resistant material, and the inner side of communicating pipe 2 is provided with the body liner 13 be made up of heat-resisting chemical resistant material;
Comprise the first body 2a be connected with regulating tank described communicating pipe 2, the the second body 2b be connected with retort 3 and be connected the first body, the adapter sleeve 21 of the second body, one end outer wall that first body is connected with the second body is provided with silk braid plug 16, on the first body and the second body, the silk braid 17 slided along respective body is provided with inside silk braid plug 16, silk braid outer wall there is the first outside screw 18, the inwall of adapter sleeve there is first internal thread 22 corresponding with the first outside screw, first body and the second body are by the first outside screw, first internal thread is together with pipe connecting spinning, flow control pad 23 has been clamped between inherent first body of adapter sleeve and the end face of the second body, there is ventilating pit 14 at flow control pad 23 center,
Described regulating tank 1 is identical with the structure of retort 3, include the shell 5 that explosion-proof metallic substance is made, tank body liner 6 and lid cover 4, shell and liner are the hollow structure of upper opening, neck bush is cased, liner upper end outer wall is provided with the seal convexity 15 compressing edge on housing mouth, lid cover 4 is the hollow structure of upper and lower opening, lid cover 4 inwall is provided with the second internal thread 9, outer shell outer wall is provided with second outside screw 10 corresponding with the second internal thread, lid cover is contained in shell upper by the second internal thread and the second external thread rotary, one end that first body is connected with regulating tank, one end that second body is connected with retort is provided with the sealing cover 11 of outwardly convex, under sealing cover is placed in lid cover and between seal convexity, be connected and sealed by screwing lid cover, integrant sealed structure,
B, by water and Zn (CH
3cOO)
2h
2o in mass ratio 16 ﹕ 25 ratio mixing add in tank body liner 6, and suspend the crystal seed of a zincite crystal in the solution, tank body liner 6 is inserted in shell 5, silk braid plug 16 one end of first body 2a is entered from lid cover 4 infraoral, upper oral part passes, sealing cover 11 on first body 2a is pressed on the seal convexity of this tank body liner, lid cover is tightened on shell, be retort 1;
C. getting with the isopyknic mass concentration of the water in steps A is 28% ammoniacal liquor, insert in another tank body liner, this tank body liner is inserted in shell, silk braid plug 16 one end of second body 2b is entered from lid cover 4 infraoral, upper oral part passes, sealing cover 11 on second body 2b is pressed on the seal convexity of this tank body liner, lid cover is tightened on shell, be regulating tank 3;
D, get flow control pad 23 and insert in adapter sleeve 21, two silk braids of the first body 2a and the second body 2b are screwed in from adapter sleeve 21 two ends respectively and compresses flow control pad;
E, retort 1 is placed in the weighing apparatus incubator of 95 DEG C-150 DEG C, regulating tank 3 is placed in alternating temperature case, maintains reaction 30-180 days, period the temperature of regulating tank 3 be warmed up to 80 DEG C from 40 DEG C, temperature is in evenly raising in units of sky;
F, taking-up retort 1 and regulating tank 3, adapter sleeve 21 of first outwarding winding after being cooled to normal temperature, then outward winding respectively retort 1 and regulating tank 3, take out the crystal of generation from retort 1.
The inventive method is novel unique, and advantages of simple, possesses the effect of synthesizing multiple inorganic crystal, and to scientific research, medical important in inhibiting, apparatus of the present invention are simple, easy to operate, effective, is technological innovation prepared by the hydrothermal method of crystal.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Fig. 2 is the structural representation of synthesizer of the present invention.
Fig. 3 is the sectional view of retort of the present invention or regulating tank.
Fig. 4 is the sectional view of communicating pipe of the present invention.
Fig. 5 is the installation sectional view at adapter sleeve place of the present invention.
Fig. 6 is the sectional view of shell of the present invention.
Fig. 7 is the sectional view of tank body liner of the present invention.
Fig. 8 is the sectional view of lid of the present invention cover.
Fig. 9 is the sectional view of adapter sleeve of the present invention.
Figure 10 is the part sectioned view of communicating pipe of the present invention.
Figure 11 is the structural representation that inventive flow controls pad.
Figure 12 is the sectional view that inventive flow controls pad.
Figure 13 is the fluorescence spectrum figure of the zincite crystal utilizing literature method to prepare.
Figure 14 is the fluorescence spectrum figure of the zincite crystal utilizing the inventive method to prepare.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Provided by Fig. 1 to Figure 12, the present invention includes regulating tank 1, communicating pipe 2 and retort 3, the inner chamber of regulating tank is through the intracavity inter-connection of communicating pipe and retort, regulating tank 1 is identical with the structure of retort 3, be airtight hollow structure, the inner chamber of the two all arranges the tank body liner 6 be made up of heat-resisting chemical resistant material, and the inner side of communicating pipe 2 is provided with the body liner 13 be made up of heat-resisting chemical resistant material;
For ensureing result of use, comprise the first body 2a be connected with regulating tank described communicating pipe 2, the the second body 2b be connected with retort 3 and be connected the first body, the adapter sleeve 21 of the second body, one end outer wall that first body is connected with the second body is provided with silk braid plug 16, on the first body and the second body, the silk braid 17 slided along respective body is provided with inside silk braid plug 16, silk braid outer wall there is the first outside screw 18, the inwall of adapter sleeve there is first internal thread 22 corresponding with the first outside screw, first body and the second body are by the first outside screw, first internal thread is together with pipe connecting spinning, flow control pad 23 has been clamped between inherent first body of adapter sleeve and the end face of the second body, there is ventilating pit 14 at flow control pad 23 center,
Described regulating tank 1 is identical with the structure of retort 3, include the shell 5 that explosion-proof metallic substance is made, tank body liner 6 and lid cover 4, shell and liner are the hollow structure of upper opening, neck bush is cased, liner upper end outer wall is provided with the seal convexity 15 compressing edge on housing mouth, lid cover 4 is the hollow structure of upper and lower opening, lid cover 4 inwall is provided with the second internal thread 9, outer shell outer wall is provided with second outside screw 10 corresponding with the second internal thread, lid cover is contained in shell upper by the second internal thread and the second external thread rotary, one end that first body is connected with regulating tank, one end that second body is connected with retort is provided with the sealing cover 11 of outwardly convex, under sealing cover is placed in lid cover and between seal convexity, be connected and sealed by screwing lid cover, integrant sealed structure,
Described silk braid 17 is provided with the one or the six rib pipe cap 19 puted forth effort for wrench, described adapter sleeve 21 is provided with the two or the six rib pipe cap 20 puted forth effort for wrench, described lid cover 4 is provided with the three or the six rib pipe cap 7 puted forth effort for wrench;
Described lid cover 4, shell 5 and the cladding material of communicating pipe 2 are explosion-proof metallic substance and make, as stainless material;
The material that described tank body liner 6, body liner 13 and flow control pad 23 are high temperature resistant resistance to chemical attack is made, as tetrafluoroethylene;
The external diameter 0.1-0.5mm less of the internal diameter of shell 5 of described tank body liner 6, makes tank body liner put into shell, does not make again have obvious gap between two walls;
The height of described tank body liner 6 equals spatial altitude in shell 5 after deducting seal convexity 15, makes tank body liner 6 put into bottom after shell 5 and contacts with outer casing inner wall, edge on the oral area that seal convexity 15 is pressed in shell 5;
Sealing cover 11 diameter of described communicating pipe 2 is less than upper shield 4 infraoral internal diameter 0.1-0.5mm, sealing cover 11 can be moved freely in upper shield 4 and can cover the seal convexity 15 of tank body liner 6 completely, not deviating from from the upper oral part 8 of upper shield 4;
Described silk braid 17 internal diameter is greater than communicating pipe 2 external diameter 0.1-0.5mm, and is less than the external diameter of silk braid plug 16, makes silk braid 17 can be free to slide on communicating pipe 2 and can not come off from silk braid plug 16;
Described silk braid plug 16 external diameter is less than the external diameter of silk braid 17, and silk braid 17 is not stopped when adapter sleeve 21 connects;
The external diameter of described silk braid 17 is less than the internal diameter connecting oral area 8 of upper shield 4, enables silk braid 17 end of communicating pipe 2 pass freely through upper shield 4;
The length of the first outside screw 18 of described silk braid 17 is more than or equal to 1/2nd of the length of adapter sleeve 21, can compress flow control pad 23 when two silk braids are entered from adapter sleeve two ends in adapter sleeve 21;
The external diameter of described flow control pad 23 is less than the internal diameter of adapter sleeve 21, and is greater than the internal diameter of communicating pipe 2, and the diameter of the ventilating pit 24 of flow control pad 23 is less than or equal to the internal diameter of communicating pipe 2.
Adopt a hydrothermal method Zinc oxide single crystal material synthesis method for synthesizer described in claim 1, it is characterized in that, comprise the following steps:
A, installation synthesizer
Synthesizer comprises regulating tank 1, communicating pipe 2 and retort 3, the inner chamber of regulating tank is through the intracavity inter-connection of communicating pipe and retort, regulating tank 1 is identical with the structure of retort 3, be airtight hollow structure, the inner chamber of the two all arranges the tank body liner 6 be made up of heat-resisting chemical resistant material, and the inner side of communicating pipe 2 is provided with the body liner 13 be made up of heat-resisting chemical resistant material;
Comprise the first body 2a be connected with regulating tank described communicating pipe 2, the the second body 2b be connected with retort 3 and be connected the first body, the adapter sleeve 21 of the second body, one end outer wall that first body is connected with the second body is provided with silk braid plug 16, on the first body and the second body, the silk braid 17 slided along respective body is provided with inside silk braid plug 16, silk braid outer wall there is the first outside screw 18, the inwall of adapter sleeve there is first internal thread 22 corresponding with the first outside screw, first body and the second body are by the first outside screw, first internal thread is together with pipe connecting spinning, flow control pad 23 has been clamped between inherent first body of adapter sleeve and the end face of the second body, there is ventilating pit 14 at flow control pad 23 center,
Described regulating tank 1 is identical with the structure of retort 3, include the shell 5 that explosion-proof metallic substance is made, tank body liner 6 and lid cover 4, shell and liner are the hollow structure of upper opening, neck bush is cased, liner upper end outer wall is provided with the seal convexity 15 compressing edge on housing mouth, lid cover 4 is the hollow structure of upper and lower opening, lid cover 4 inwall is provided with the second internal thread 9, outer shell outer wall is provided with second outside screw 10 corresponding with the second internal thread, lid cover is contained in shell upper by the second internal thread and the second external thread rotary, one end that first body is connected with regulating tank, one end that second body is connected with retort is provided with the sealing cover 11 of outwardly convex, under sealing cover is placed in lid cover and between seal convexity, be connected and sealed by screwing lid cover, integrant sealed structure,
B, by water and Zn (CH
3cOO)
2h
2o in mass ratio 16 ﹕ 25 ratio mixing add in tank body liner 6, and suspend the crystal seed of a zincite crystal in the solution, tank body liner 6 is inserted in shell 5, silk braid plug 16 one end of first body 2a is entered from lid cover 4 infraoral, upper oral part passes, sealing cover 11 on first body 2a is pressed on the seal convexity of this tank body liner, lid cover is tightened on shell, be retort 1;
C. getting with the isopyknic mass concentration of the water in steps A is 28% ammoniacal liquor, insert in another tank body liner, this tank body liner is inserted in shell, silk braid plug 16 one end of second body 2b is entered from lid cover 4 infraoral, upper oral part passes, sealing cover 11 on second body 2b is pressed on the seal convexity of this tank body liner, lid cover is tightened on shell, be regulating tank 3;
D, get aperture 0.1mm flow control pad 23 and insert in adapter sleeve 21, two silk braids of the first body 2a and the second body 2b are screwed in from adapter sleeve 21 two ends respectively and compresses flow control pad;
E, retort 1 is placed in the weighing apparatus incubator of 95 DEG C-150 DEG C, regulating tank 3 is placed in alternating temperature case, maintains reaction 30-180 days, period the temperature of regulating tank 3 be warmed up to 80 DEG C from 40 DEG C, temperature is in evenly raising in units of sky;
F, taking-up retort 1 and regulating tank 3, adapter sleeve 21 of first outwarding winding after being cooled to normal temperature, then outward winding respectively retort 1 and regulating tank 3, take out the crystal of generation from retort 1.
The process that balances each other being changed to ammoniacal liquor mixed system in described regulating tank 3, equation is:
Return the vapor-liquid equilibrium data of ammoniacal liquor mixed system, the semi empirical calculation formula that can obtain institute's ammonia vapour pressure is:
lnp
NH3＝20.9736-4311.2/T+lnx
NH3+[12.3134-0.03067·T]·x
NH3
In preparation process, along with ammonia effusion and react with the zinc acetate in retort 1, the ammonia concn in regulating tank 3 is reducing gradually, i.e. x
nH3reducing gradually, according to semi empirical calculation formula, this can cause the ammonia saturated vapor pressure in communicating pipe 2 to reduce, and namely pNH3 reduces, and this can cause again the ammonia being transferred to retort 1 from regulating tank 3 to reduce, and speed of reaction is diminished, affects the crystallization of crystal.And as can be seen from semi empirical calculation formula, raised temperature can make ammonia saturated vapor pressure raise, therefore, the temperature raising regulating tank 3 can offset the impact of concentration reduction on ammonia gas vapor pressure.So the control of regulating tank 3 temperature is an alternating temperature process from low to high in building-up process.
Reaction in described retort 1 is as follows:
2OH
－+Zn
2+＝Zn(OH)
2
Control to overflow the speed of ammonia from regulating tank 3, just can control the speed of response of ammonia and zinc acetate in retort 1, also the crystallization velocity of zincite crystal is just controlled, the crystallization finally making zinc oxide energy stable is on the dominant growth face of crystal seed, form monocrystalline, the inventive method possesses the function of synthesizing multiple crystal, many kinds of parameters can be regulated in building-up process, easy to operate, easy to use, effective, can be used for the aspect such as commercial production, scientific research, there is good Social and economic benef@, through testing the identical or akin test effect all obtained:
Applicant utilizes (as: Dong Guoyi in document, Wei Zhiren, Lin Yan, Wang Liming, Li Zhiqiang, Zhang Huawei, hydrothermal Synthesis of ZnO crystal, artificial lens journal, 2003,32 (2): 130-133.) conventional hydrothermal Synthesis of ZnO crystal is prepared zincite crystal with use the inventive method and is contrasted, the crystal maximum diameter utilizing literature method to prepare is 5 μm, and length is 40 μm, and the crystal diameter using the inventive method to prepare reaches 5mm, length, close to 1cm, is far longer than the crystalline size of literature method gained.Crystal mass spectrophotofluorometer measures, and as shown in Figure 13,14, in figure, X-coordinate Wavelength represents wavelength, and ordinate zou Intensity represents intensity;
As can be seen from Figure 13,14, two crystal all have a narrow excitation peak at 380nm place, for the peak that the intrinsic excitation light of zincite crystal produces, but in Figure 13, namely with the peak that the zincite crystal that literature method obtains has a peak width at half height very wide at 510nm place, and intensity is very large, and peak is herein the deep energy level excitation peak that zincite crystal defect produces, and Figure 14, the peak that the zincite crystal namely utilizing the present invention to obtain only has level weak at 510nm place.Two figure compare, peak value B figure at 380nm place than A figure weak 3%, and at 510nm place B figure is 20 times of A figure, therefore can illustrate, when two crystal intrinsic excitations are substantially the same, the zincite crystal utilizing the present invention to prepare is far smaller than the obtained zincite crystal of literature method.Illustrate that the perfect degree of the crystallization of the zincite crystal utilizing the inventive method to prepare is greatly improved.
Claims (5)
1. a hydrothermal method Zinc oxide single crystal materials synthesis device, it is characterized in that, comprise regulating tank (1), communicating pipe (2) and retort (3), the inner chamber of regulating tank is through the intracavity inter-connection of communicating pipe and retort, regulating tank (1) is identical with the structure of retort (3), be airtight hollow structure, the inner chamber of the two all arranges the tank body liner (6) be made up of heat-resisting chemical resistant material, and the inner side of communicating pipe (2) is provided with the body liner (13) be made up of heat-resisting chemical resistant material.
2. hydrothermal method Zinc oxide single crystal materials synthesis device according to claim 1, it is characterized in that, described communicating pipe (2) comprises the first body (2a) be connected with regulating tank, with retort (3) be connected the second body (2b) and be connected the first body, the adapter sleeve (21) of the second body, one end outer wall that first body is connected with the second body is provided with silk braid plug (16), silk braid plug (16) inner side is provided with the silk braid (17) slided along respective body on the first body and the second body, silk braid outer wall there is the first outside screw (18), the inwall of adapter sleeve there is first internal thread (22) corresponding with the first outside screw, first body and the second body are by the first outside screw, first internal thread is together with pipe connecting spinning, flow control pad (23) has been clamped between inherent first body of adapter sleeve and the end face of the second body, there is ventilating pit (14) at flow control pad (23) center.
3. hydrothermal method Zinc oxide single crystal materials synthesis device according to claim 2, it is characterized in that, described regulating tank (1) is identical with the structure of retort (3), include the shell (5) that explosion-proof metallic substance is made, tank body liner (6) and lid cover (4), shell and liner are the hollow structure of upper opening, neck bush is cased, liner upper end outer wall is provided with the seal convexity (15) compressing edge on housing mouth, the hollow structure that lid cover (4) is upper and lower opening, lid cover (4) inwall is provided with the second internal thread (9), outer shell outer wall is provided with second outside screw (10) corresponding with the second internal thread, lid cover is contained in shell upper by the second internal thread and the second external thread rotary, one end that first body is connected with regulating tank, one end that second body is connected with retort is provided with the sealing cover (11) of outwardly convex, under sealing cover is placed in lid cover and between seal convexity, be connected and sealed by screwing lid cover, integrant sealed structure.
4. hydrothermal method Zinc oxide single crystal materials synthesis device according to claim 3, it is characterized in that, described silk braid (17) is provided with the one or the six rib pipe cap (19) puted forth effort for wrench, described adapter sleeve (21) is provided with the two or the six rib pipe cap (20) puted forth effort for wrench, described lid cover (4) is provided with the three or the six rib pipe cap (7) puted forth effort for wrench.
5. adopt a hydrothermal method Zinc oxide single crystal material synthesis method for synthesizer described in claim 1, it is characterized in that, comprise the following steps:
A, installation synthesizer
Synthesizer comprises regulating tank (1), communicating pipe (2) and retort (3), the inner chamber of regulating tank is through the intracavity inter-connection of communicating pipe and retort, regulating tank (1) is identical with the structure of retort (3), be airtight hollow structure, the inner chamber of the two all arranges the tank body liner (6) be made up of heat-resisting chemical resistant material, and the inner side of communicating pipe (2) is provided with the body liner (13) be made up of heat-resisting chemical resistant material;
Described communicating pipe (2) comprises the first body (2a) be connected with regulating tank, with retort (3) be connected the second body (2b) and be connected the first body, the adapter sleeve (21) of the second body, one end outer wall that first body is connected with the second body is provided with silk braid plug (16), silk braid plug (16) inner side is provided with the silk braid (17) slided along respective body on the first body and the second body, silk braid outer wall there is the first outside screw (18), the inwall of adapter sleeve there is first internal thread (22) corresponding with the first outside screw, first body and the second body are by the first outside screw, first internal thread is together with pipe connecting spinning, flow control pad (23) has been clamped between inherent first body of adapter sleeve and the end face of the second body, there is ventilating pit (14) at flow control pad (23) center,
Described regulating tank (1) is identical with the structure of retort (3), include the shell (5) that explosion-proof metallic substance is made, tank body liner (6) and lid cover (4), shell and liner are the hollow structure of upper opening, neck bush is cased, liner upper end outer wall is provided with the seal convexity (15) compressing edge on housing mouth, the hollow structure that lid cover (4) is upper and lower opening, lid cover (4) inwall is provided with the second internal thread (9), outer shell outer wall is provided with second outside screw (10) corresponding with the second internal thread, lid cover is contained in shell upper by the second internal thread and the second external thread rotary, one end that first body is connected with regulating tank, one end that second body is connected with retort is provided with the sealing cover (11) of outwardly convex, under sealing cover is placed in lid cover and between seal convexity, be connected and sealed by screwing lid cover, integrant sealed structure,
B, by water and Zn (CH
3cOO)
2h
2o in mass ratio 16 ﹕ 25 ratio mixing add in tank body liner (6), and suspend the crystal seed of a zincite crystal in the solution, tank body liner (6) is inserted in shell 5, silk braid plug (16) one end of first body (2a) is entered from lid cover (4) infraoral, upper oral part passes, sealing cover (11) on first body (2a) is pressed on the seal convexity of this tank body liner, lid cover is tightened on shell, is retort (1);
C. getting with the isopyknic mass concentration of the water in steps A is 28% ammoniacal liquor, insert in another tank body liner, this tank body liner is inserted in shell, silk braid plug (16) one end of second body (2b) is entered from lid cover (4) infraoral, upper oral part passes, sealing cover (11) on second body (2b) is pressed on the seal convexity of this tank body liner, lid cover is tightened on shell, be regulating tank (3);
D, get flow control pad (23) and insert in adapter sleeve (21), two silk braids of the first body (2a) and the second body (2b) are screwed in from adapter sleeve (21) two ends respectively and compress flow control pad;
E, retort (1) is placed in the weighing apparatus incubator of 95 DEG C-150 DEG C, regulating tank (3) is placed in alternating temperature case, maintain reaction 30-180 days, the temperature of period regulating tank (3) is warmed up to 80 DEG C from 40 DEG C, and temperature is in evenly raising in units of sky;
F, taking-up retort (1) and regulating tank (3), first to outward winding after being cooled to normal temperature adapter sleeve (21), retort of outwarding winding respectively again (1) and regulating tank (3), take out the crystal generated from retort (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610137960.1A CN105568360B (en) | 2016-03-10 | 2016-03-10 | Hydro-thermal method Zinc oxide single crystal materials synthesis device and synthetic method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610137960.1A CN105568360B (en) | 2016-03-10 | 2016-03-10 | Hydro-thermal method Zinc oxide single crystal materials synthesis device and synthetic method |
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| Publication Number | Publication Date |
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| CN105568360A true CN105568360A (en) | 2016-05-11 |
| CN105568360B CN105568360B (en) | 2017-11-24 |
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| JP2003095790A (en) * | 2001-09-21 | 2003-04-03 | Tokyo Denpa Co Ltd | Method of preparing seed crystal of zinc oxide and method of growing single crystal of zinc oxide |
| US7279040B1 (en) * | 2005-06-16 | 2007-10-09 | Fairfield Crystal Technology, Llc | Method and apparatus for zinc oxide single crystal boule growth |
| CN101983263A (en) * | 2008-04-04 | 2011-03-02 | 株式会社福田结晶技术研究所 | Zinc oxide single crystal and method for producing the same |
| CN102489236A (en) * | 2011-11-17 | 2012-06-13 | 四川嘉宝莉涂料有限公司 | Liquid granite paint production device |
| US8557628B2 (en) * | 2010-10-07 | 2013-10-15 | Fairfield Crystal Technology, Llc | Method for production of zinc oxide single crystals |
| CN205387602U (en) * | 2016-03-10 | 2016-07-20 | 河南工程学院 | Hydrothermal method zinc oxide single crystal material synthesizer |
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| JP2003095790A (en) * | 2001-09-21 | 2003-04-03 | Tokyo Denpa Co Ltd | Method of preparing seed crystal of zinc oxide and method of growing single crystal of zinc oxide |
| US7279040B1 (en) * | 2005-06-16 | 2007-10-09 | Fairfield Crystal Technology, Llc | Method and apparatus for zinc oxide single crystal boule growth |
| CN101983263A (en) * | 2008-04-04 | 2011-03-02 | 株式会社福田结晶技术研究所 | Zinc oxide single crystal and method for producing the same |
| US8557628B2 (en) * | 2010-10-07 | 2013-10-15 | Fairfield Crystal Technology, Llc | Method for production of zinc oxide single crystals |
| CN102489236A (en) * | 2011-11-17 | 2012-06-13 | 四川嘉宝莉涂料有限公司 | Liquid granite paint production device |
| CN205387602U (en) * | 2016-03-10 | 2016-07-20 | 河南工程学院 | Hydrothermal method zinc oxide single crystal material synthesizer |
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