CN106192012B - A kind of high dielectric constant diisopropylamine nitrate organic crystal and its growing method - Google Patents
A kind of high dielectric constant diisopropylamine nitrate organic crystal and its growing method Download PDFInfo
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- CN106192012B CN106192012B CN201610807845.0A CN201610807845A CN106192012B CN 106192012 B CN106192012 B CN 106192012B CN 201610807845 A CN201610807845 A CN 201610807845A CN 106192012 B CN106192012 B CN 106192012B
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- diisopropylamine
- crystal
- dielectric constant
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- nitrate
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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
- C30B29/54—Organic compounds
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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
- C30B7/08—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by cooling of the solution
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- Crystallography & Structural Chemistry (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of high dielectric constant diisopropylamine nitrate organic crystal and its growing methods, belong to monoclinic system, space group P21/ n, cell parameter are a=8.1799, b=8.3530, c=14.3808, α=γ=90.00 °, β=96.72 °.Diisopropylamine nitrate organic crystal is grown using seed crystal solution-evaporation at room temperature, obtained organic crystal is having a size of 11mm × 5mm × 3mm, by test crystal Jie's temperature spectrum, it is found that the crystal has very high dielectric constant, which can be applied to the fields such as capacitor.
Description
Technical field
The present invention relates to a kind of high dielectric constant diisopropylamine nitrate organic crystal and its growing methods.
Background technique
With the rapid development of electronic technology, capacitor is required to develop to miniaturization, high performance, lightness direction, this
Require corresponding dielectric substance that there is higher dielectric constant, lower dielectric loss, better mechanical performance.Although pottery
Porcelain dielectric substance has very excellent dielectric properties, but ceramic capacitor needs to be sintered in the fabrication process, consumption
Can be big, complex process, and also the flexibility of this dielectric material is poor, and it can when being subjected to mechanical impact or violent temperature change
It can crack, affect the use of capacitor.High dielectric constant diisopropylamine nitrate organic crystal preparation process energy-saving ring
It protects, light quality, and there is good mechanical-stretching property.Very big development potentiality will be had in capacitor direction.
Summary of the invention
The purpose of the present invention is to provide a kind of high dielectric constant diisopropylamine nitrate organic crystal and its growing methods.
A kind of high dielectric constant diisopropylamine nitrate organic crystal, it is characterised in that：Crystal be it is colorless and transparent, work as frequency
When for 0.1MHz, temperature is relative dielectric constant 5348 at 166 DEG C, and when frequency is 1MHz, temperature is at 166 DEG C, relatively
Dielectric constant is 4040.
Technical scheme is as follows：
The present invention provides a kind of preparation method of high dielectric constant diisopropylamine nitrate organic crystal compound, step
It is as follows：Using diisopropylamine and nitric acid as raw material, molar ratio 1:1, it is at room temperature that diisopropylamine is soluble in water, in magnetic agitation
Under continuous, nitric acid is slowly added into diisopropylamine solution, is placed in an oven at 60 DEG C 8 ~ 16 hours, places room temperature,
It using capillary contact solution surface, has tiny colourless transparent crystal and generates, which is diisopropylamine nitrate chemical combination
Object.
A kind of organic crystal of high dielectric constant provided by the invention, its chemical name is diisopropylamine nitrate, belong to
Monoclinic system, space group P21/ n, cell parameter be a=8.1799, b=8.3530, c=14.3808, α=γ=
90.00 °, β=96.72 °, V=975.82.
A kind of growing method of high dielectric constant diisopropylamine nitrate organic crystal provided by the invention, step is such as
Under：
Step 1：Diisopropylamine is measured at room temperature, it is mutually dissolved in beaker with deionized water；
Step 2：Measurement mass fraction is 68% nitric acid solution, in the case where magnetic agitation, by the nitric acid solution of measurement
It using dropping funel, is slowly dropped into the beaker for filling diisopropylamine liquid, is added dropwise, stand solution；
Step 3：By preparation ground solution in step 1, it is put into baking oven, is dried 8~16 hours under the conditions of 60 DEG C, takes out and burns
Cup is placed into room temperature, reaches diisopropylamine nitrate solution saturation point, one end of capillary is inserted into solution, solution table
The broken grain for having naked eyes that can see on face, these broken grains regard seed crystal, beaker are shut with preservative film, and capillary is used on preservative film
Pipe pricks 5~10 holes, places 4~10 days, the diisopropylamine nitrate organic crystal with high dielectric constant can be obtained；
Wherein, the mass ratio of the material value of diisopropylamine and ionized water is 1 in step 1:3, nitric acid and diisopropyl in step 2
It is 1 that amine the mass ratio of the material value, which is the mass ratio of the material value,:1.
The beneficial effects of the present invention are
(1) large scale diisopropylamine nitric acid single-crystal of salt is grown, and has successfully parsed the cell parameter of the crystal；
(2) diisopropylamine nitrate organic crystal is tested, finds it with good dielectric properties.
Detailed description of the invention
Fig. 1 is the photo of diisopropylamine nitrate organic crystal of the present invention；
Fig. 2 is the powder xrd pattern of diisopropylamine nitrate organic crystal of the present invention；
Fig. 3 is the monocrystalline XRD diagram of diisopropylamine nitrate organic crystal of the present invention；
Fig. 4 is Jie's temperature map of diisopropylamine nitrate organic crystal of the present invention.
Specific embodiment
Embodiment 1
Diisopropylamine nitric acid salt crystal is grown using seed crystal solution-evaporation at room temperature, compound is synthesized using aqua-solution method
Diisopropylamine nitrate：Raw materials used diisopropylamine is that analysis is pure, measures 26ml, and concentration is 65% nitric acid, measures 10ml, then
15ml deionized water is being measured, diisopropylamine and the water of measurement are being dissolved each other, in the case where being stirred continuously, by the nitre of measurement
Acid solution uses dropping funel, is slowly dropped into the beaker for filling diisopropylamine liquid, is added dropwise, and stands solution.More than
Operating procedure is multiple, and the beaker used is 100ml, and preparation ground solution is put into baking oven, dries 8~16 hours under the conditions of 60 DEG C,
Beaker is taken out, room temperature is placed into, diisopropylamine nitrate solution saturation point is reached, one end of capillary is inserted into solution,
The broken grain for having naked eyes that can see in solution surface, these broken grains regard seed crystal, beaker are shut with preservative film, and makes on preservative film
5~10 holes are pricked with capillary, are placed 4~10 days, when organism precipitation but is not monocrystalline, can use recrystallization technology,
Repeated crystallization is carried out, the diisopropylamine nitrate organic crystal with high dielectric constant, 11mm × 5 of the crystal can be obtained
Mm × 3mm (Fig. 1).Prepared monocrystalline is tested using monocrystalline XRD diffractometer, and obtained data are solved
Analysis, obtains diisopropylamine nitrate cell parameter, and simulation obtains diisopropylamine nitrate XRD diffracting spectrum (Fig. 3).
Embodiment 2
Compound diisopropylamine nitrate is synthesized using aqua-solution method：Raw materials used diisopropylamine is to analyze pure, measurement
26ml, nitric acid are concentrated nitric acid, measure 10ml, are then measuring 5ml deionized water, diisopropylamine and the water of measurement are carried out mutual
It is molten, in the case where being stirred continuously, the nitric acid solution of measurement is used into dropping funel, is slowly dropped into and fills diisopropylamine liquid
Beaker in, be added dropwise, stand solution.By the end thereof contacts solution surface of capillary, a large amount of crystal are being had within an hour
It generates, crystal grinding will be generated, air-dried, obtaining white powder is diisopropylamine nitrate compound.
Diisopropylamine nitric acid salt powder is tested using powder X-ray RD diffractometer, resulting isopropylamine nitrate XRD spreads out
Map (Fig. 2) is penetrated, the XRD spectrum (Fig. 3) being fitted with the data that monocrystalline XRD diffractometer is measured matches.Illustrate resulting powder
For pure diisopropylamine nitrate phase.
Embodiment 3
Resulting diisopropylamine nitric acid single-crystal of salt is handled, monocrystalline shape rectangular shape is made, by the two of monocrystalline
A opposite face coats silver paste, and guarantees that two faces are all conductive, then carries out the temperature test that is situated between, and test result is shown, diisopropylamine
Nitric acid salt crystal has high dielectric constant.
Claims (2)
1. a kind of high dielectric constant diisopropylamine nitrate organic crystal, it is characterised in that：Belong to monoclinic system, space group is
P21/ n, cell parameter are α=γ=90.00 °, β=96.72 °,
V=975.82；Crystal be it is colorless and transparent, when frequency be 0.1MHz when, temperature be 166 DEG C at, relative dielectric constant 5348, when
When frequency is 1MHz, temperature is relative dielectric constant 4040 at 166 DEG C.
2. a kind of growing method of high dielectric constant diisopropylamine nitrate organic crystal as described in claim 1, feature
Seed crystal solution-evaporation is being used to grow crystal at room temperature, specific step is as follows：
Step 1：Diisopropylamine is measured at room temperature, it is mutually dissolved in beaker with deionized water；
Step 2：Measurement mass fraction is 68% nitric acid solution, and in the case where magnetic agitation, the nitric acid solution of measurement is used
Dropping funel is slowly dropped into the beaker for filling diisopropylamine liquid, is added dropwise, and stands solution；
Step 3：The solution that will be prepared in step 1, is put into baking oven, dries 8~16 hours under the conditions of 60 DEG C, takes out beaker, puts
Room temperature is set, diisopropylamine nitrate solution saturation point is reached, one end of capillary is inserted into solution, is had in solution surface
The broken grain that naked eyes can be seen, these broken grains regard seed crystal, beaker are shut with preservative film, and prick 5 using capillary on preservative film
~10 holes place 4~10 days, the diisopropylamine nitrate organic crystal with high dielectric constant can be obtained；
Wherein the mass ratio of the material value of diisopropylamine and deionized water is 1 in step 1：3, nitric acid and diisopropylamine in step 2
The mass ratio of the material value be 1：1.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921196A (en) * | 2009-06-10 | 2010-12-22 | 宁波大学 | Organic amine phosphate nonlinear optical crystal [C6H9N3O2][HPO4] |
| CN102337593A (en) * | 2010-12-22 | 2012-02-01 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal 1-ethyl-3-methylimidazol lead tribromide and growing method thereof |
| CN103088424A (en) * | 2011-11-01 | 2013-05-08 | 中国科学院新疆理化技术研究所 | Compound sodium borate monohydrate nonlinear optical crystal, and preparation method and application thereof |
| CN104630875A (en) * | 2015-01-27 | 2015-05-20 | 东南大学 | Novel environment-friendly and energy-saving growth method of large-sized blocky information storage ferroelectric single crystals |
| CN105862120A (en) * | 2016-03-29 | 2016-08-17 | 东南大学 | Growth method for large-size information storage monocrystals |
-
2016
- 2016-09-07 CN CN201610807845.0A patent/CN106192012B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921196A (en) * | 2009-06-10 | 2010-12-22 | 宁波大学 | Organic amine phosphate nonlinear optical crystal [C6H9N3O2][HPO4] |
| CN102337593A (en) * | 2010-12-22 | 2012-02-01 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal 1-ethyl-3-methylimidazol lead tribromide and growing method thereof |
| CN103088424A (en) * | 2011-11-01 | 2013-05-08 | 中国科学院新疆理化技术研究所 | Compound sodium borate monohydrate nonlinear optical crystal, and preparation method and application thereof |
| CN104630875A (en) * | 2015-01-27 | 2015-05-20 | 东南大学 | Novel environment-friendly and energy-saving growth method of large-sized blocky information storage ferroelectric single crystals |
| CN105862120A (en) * | 2016-03-29 | 2016-08-17 | 东南大学 | Growth method for large-size information storage monocrystals |
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