US3352906A - Habit modification and preparation of single crystal triglycine sulfate - Google Patents
Habit modification and preparation of single crystal triglycine sulfate Download PDFInfo
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- US3352906A US3352906A US256175A US25617563A US3352906A US 3352906 A US3352906 A US 3352906A US 256175 A US256175 A US 256175A US 25617563 A US25617563 A US 25617563A US 3352906 A US3352906 A US 3352906A
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- 239000013078 crystal Substances 0.000 title claims description 108
- GZXOHHPYODFEGO-UHFFFAOYSA-N triglycine sulfate Chemical compound NCC(O)=O.NCC(O)=O.NCC(O)=O.OS(O)(=O)=O GZXOHHPYODFEGO-UHFFFAOYSA-N 0.000 title claims description 60
- 108010067216 glycyl-glycyl-glycine Proteins 0.000 title claims description 52
- 238000012986 modification Methods 0.000 title claims description 16
- 230000004048 modification Effects 0.000 title claims description 16
- 238000002360 preparation method Methods 0.000 title claims description 7
- 239000000243 solution Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 17
- 239000012535 impurity Substances 0.000 claims description 8
- XKUKSGPZAADMRA-UHFFFAOYSA-N glycyl-glycyl-glycine Chemical compound NCC(=O)NCC(=O)NCC(O)=O XKUKSGPZAADMRA-UHFFFAOYSA-N 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000012047 saturated solution Substances 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 9
- 239000000975 dye Substances 0.000 description 6
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical class OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910001417 caesium ion Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 Tl+ ions Chemical class 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 229910001413 alkali metal ion Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910001419 rubidium ion Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- MFPXBAPCIMYWHZ-UHFFFAOYSA-N 2-aminoacetic acid;selenic acid Chemical compound NCC(O)=O.O[Se](O)(=O)=O MFPXBAPCIMYWHZ-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 125000000853 cresyl group Chemical group C1(=CC=C(C=C1)C)* 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910001412 inorganic anion Inorganic materials 0.000 description 1
- 229910001411 inorganic cation Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- RBDJQFKUZPMOFH-UHFFFAOYSA-I pentasodium;3-amino-4-[[4-[4-[(2-amino-3,6-disulfonatonaphthalen-1-yl)diazenyl]-3-sulfonatophenyl]phenyl]diazenyl]naphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].C12=CC=C(S([O-])(=O)=O)C=C2C=C(S([O-])(=O)=O)C(N)=C1N=NC1=CC=C(C=2C=C(C(N=NC=3C4=CC=C(C=C4C=C(C=3N)S([O-])(=O)=O)S([O-])(=O)=O)=CC=2)S([O-])(=O)=O)C=C1 RBDJQFKUZPMOFH-UHFFFAOYSA-I 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G7/00—Capacitors in which the capacitance is varied by non-mechanical means; Processes of their manufacture
- H01G7/02—Electrets, i.e. having a permanently-polarised dielectric
- H01G7/021—Electrets, i.e. having a permanently-polarised dielectric having an organic dielectric
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/02—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length in solution
Definitions
- the present invention relates to the method of growing crystals and more particularly to crystal growth with controlled habit modification of triglycine sulfate by means of monovalent cations.
- a main purpose of this invention is the growth, from an aqueous solution of triglycine sulfate and deuterium doped triglycine sulfate, of single crystals having a particularly highly desirable crystal habit for use in the fabrication of better ferroelectric memory elements as well as ferroelectric capacitors and dielectric modulators.
- the present invention is a significant development in the growing of crystals having a prefered crystallographic orientation for the fabrication of ferroelectric memory matrices.
- the present method of growing crystals allows about 60 to 70 percent of the crystal to be used successfully for building small ferroelectric matrices. This method is not restricted to triglycine sulfate but may prove to be useful for isomorphous crystalline solids.
- Another object of the invention is to provide crystal growth with controlled habit modification by means of monovalent cations.
- Still another object of the invention is to provide growth of single crystal plates with low dispersion of the ferroelectric axis.
- FIG. 1 is an illustration of a typical triglycine sulfate.
- FIG. 2 is an illustration of a typical triglycine sulfate crystal grown by the present method with controlled modification of the external habit as shown.
- FIG. 3 is an edge view of the thin flat crystal shown in FIG. 2 and also illustrating the seed crystal and mounting rod.
- the typical crystal of triglycine sulfate grown from aqueous solution has an external habit as shown.
- the crystallographic axes are labelled for a crystal having such a habit.
- the axes shown are normal nomenclature for monoclinic crystals.
- the labeling of the axes is consistent with the class of monoclinic crystals as tabulated in 'Danas Manual of Mineralogy, Wiley (1959). It is well known that in triglycine sulfate the b-axis is the ferroelectric axis.
- the method of the present invention is for the modification of the external habit of triglycine sulfate and deuterated triglycine sulfate crystals in order to obtain crystals which grow uniformly in all directions except the crystallographic [001] direction, along the C-axis.
- the thickness of the crystals grOWn by the present method depends upon the thickness of the original seed crystal; a negligible, less than 1 percent, growth occurs in the [001] direction, along the C-axis; thus thin single crystal plates of the order of 1 millimeter to 1 centimeter thickness can be obtained. Thin single crystal plates of more than three inches in diameter have been grown by this method such as shown in FIGS. 2 and 3.
- a small seed crystal having the desired thickness is drilled and mounted on a glass rod so that the [101] faces of the crystal are perpendicular to the rod.
- the seed is then planted in a glass container containing approximately 1400 ml. of saturated solution containing the required impurity addition at a temperature of 0.1 to 1.0 C. above the saturation temperature.
- the glass container is immersed in a water bath controlled to i0.02 C. by means of a magnetic set, mercury thermoregulator and a sensitive electronic relay.
- the temperature is programmed down at rates varying from 02 C. to 0.5 C. per day until the crystal reaches the desired size. Agitation within the solution is achieved by means of a magnetic stirrer.
- the dyes used included Niagara Sky Blue BB,v Buffalo Black NBR, Trypan Red, Congo Red and Brilliant Cresyl Blue. Only minor habit modifications were obtained with any of the above dyes, and none were of practical application. Mechanical methods of inhibiting growth could be employed, such as placing the seed between glass plates, but this would conceivably lead to serious problems in obtaining uniform growth because of the difficulty of circulating the solution uniformly about the seed.
- This invention the controlled habit modification of triglycine sulfate and deuterated triglycine sulfate by means of monovalent cations, has resulted in low dispersion of the ferroelectric axis in single crystal plates thus grown and has permitted the fabrication of uniform thin sections from these plates, in turn permit-ting the building of ferroelectric devices with greater uniformity of electrical properties and simplicity of fabrication and construction.
- a method for habit modification and preparation of relatively large but thin single crystal plates of triglycine sulfate and deuterated triglycine sulfate having highly desirable crystal habit for use in ferroelectric devices comprising:
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Description
Nov. 14. 1967 c. R. PARKERSON ETAL 3,
HABIT MODIFICATION AND PREPARATION OF SINGLE CRYSTAL TRIGLYCINE SULFATE Filed Feb. 4. 1963 ATTORNEY United States Patent 3,352,906 HABIT MODIFICATION AND PREPARATION OF SINGLE CRYSTAL TRIGLYCINE SULFATE Charles R. Parkerson, Arlington, and Harry H. Wieder,
Riverside, Calif., assignors to the United States of America as represented by the Secretary of the Navy Filed Feb. 4, 1963, Ser. No. 256,175 4 Claims. (Cl. 260--534) The invention herein described may be manufactured and used by or for the Government of the United States of America for governmental purposes Without the payment of any royalities thereon or therefor.
The present invention relates to the method of growing crystals and more particularly to crystal growth with controlled habit modification of triglycine sulfate by means of monovalent cations.
A main purpose of this invention is the growth, from an aqueous solution of triglycine sulfate and deuterium doped triglycine sulfate, of single crystals having a particularly highly desirable crystal habit for use in the fabrication of better ferroelectric memory elements as well as ferroelectric capacitors and dielectric modulators.
Ferroelectricity in triglycine sulfate was discovered by Matthias et al., Physical Review, 104, 849 (1956). In order to prepare ferroelectric memory elements or other devices it is necessary to cleave a parent crystal in a direction perpendicular to the ferroelectric axis and thereafter apply electrodes of evaporated gold or silver to opposite faces of the thin laminae cleaved therefrom. Generally, the electrode areas are of the order of one square millimeter. Crystals of triglycine sulfate grown from aqueous solution have an external habit, and, in view of the large size of a parent crystal, it is difficult to cleave homogenous sections without cleavage steps. Further, in many applications it is also desirable to construct a series of ferroelectric memory elements on a series of slabs having identical geometry, and this requires additional processing of cleaved specimens.
In many cases the existence of an angular dispersion of the ferroelectric axis in crystals of triglycine sulfate has made the crystals unsuitable for device applications. Growth of triglycine sulfate crystals by the usual prior known methods is generally not satisfactory because of problems in uniformity, or ferroelectric activity which limits the use of the grown crystal volume to about percent of its total due to dispersion of the ferroelectric axes.
The present invention is a significant development in the growing of crystals having a prefered crystallographic orientation for the fabrication of ferroelectric memory matrices. The present method of growing crystals allows about 60 to 70 percent of the crystal to be used successfully for building small ferroelectric matrices. This method is not restricted to triglycine sulfate but may prove to be useful for isomorphous crystalline solids.
It is an object of the invention therefore to provide a novel method for growing ferroelectric crystals.
It is a further object of the invention to provide a novel method of growing crystals having greater uniformity.
Another object of the invention is to provide crystal growth with controlled habit modification by means of monovalent cations.
Still another object of the invention is to provide growth of single crystal plates with low dispersion of the ferroelectric axis.
Other objects and many of the attendant advantages of this invention will become readily appreciated as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings wherein:
3,352,536 Patented Nov. 14, 1967 FIG. 1 is an illustration of a typical triglycine sulfate.
crystal grown by prior known method from aqueous solution and having a normal external habit as shown, and labelled with crystallographic axes.
FIG. 2 is an illustration of a typical triglycine sulfate crystal grown by the present method with controlled modification of the external habit as shown.
FIG. 3 is an edge view of the thin flat crystal shown in FIG. 2 and also illustrating the seed crystal and mounting rod.
As illustrated in FIG. 1, the typical crystal of triglycine sulfate grown from aqueous solution has an external habit as shown. The crystallographic axes are labelled for a crystal having such a habit. The axes shown are normal nomenclature for monoclinic crystals. The labeling of the axes is consistent with the class of monoclinic crystals as tabulated in 'Danas Manual of Mineralogy, Wiley (1959). It is well known that in triglycine sulfate the b-axis is the ferroelectric axis.
The method of the present invention is for the modification of the external habit of triglycine sulfate and deuterated triglycine sulfate crystals in order to obtain crystals which grow uniformly in all directions except the crystallographic [001] direction, along the C-axis. The thickness of the crystals grOWn by the present method depends upon the thickness of the original seed crystal; a negligible, less than 1 percent, growth occurs in the [001] direction, along the C-axis; thus thin single crystal plates of the order of 1 millimeter to 1 centimeter thickness can be obtained. Thin single crystal plates of more than three inches in diameter have been grown by this method such as shown in FIGS. 2 and 3. These thin plates are easily cleaved into sections by the application of transientv pressure in the direction perpendicular to the b-axis. The b-axis, or crystallographic [010] direction lies in the plane of the crystal plate and its direction within the plate has a much smaller dispersion than in triglycine sulfate crystals having the normal (unmodified) habit.
The electrical properties of crystal laminae obtained from habit modified triglycine crystals of the present invention show that they are essentially identical to those of the normal habit; however, a much smaller angular dispersion of the ferroelectric axis (b-axis), was found within each group as compared to that of normal habit triglycine sulfate. In addition, the simplified method of preparing a ferroelectric memory element apparently leads to a smaller number of dislocations or other defects induced during the usual cutting, cleaving, grinding and polishing of the normal habit triglycine sulfate crystal.
Details of growing the modified habit triglycine sulfate are as follows:.
It was found while attempting to dope triglycine sulfate with Tl+ that the crystal habit was very much affected by the presence of this ion when there is 1 gm.-atom Tl+ per 6.13 gm.-mols of triglycine sulfate in solution (10.3 gm. Tl+ per gm. triglycine sulfate in solution). The triglycine sulfate grows as thin plates on the [101] plane of the orystal. Seed crystals planted in this solution assume essentially two dimensional growth.
No attempt has been made to determine the exact concentration of TH ion at which this effect on crystal habit begins to take place. It was found, however, that the effect is not present at a concentration as low as 1 gm.- atom Tl+: 1235 gm.-mols triglycine sulfate in solution (0.053 gm. Tl+zl00 gm. triglycine sulfate in solution). The maximum effect is still present at 1 gm.-atom Tl+:l2.26 gm.-mols triglycine sulfate in solution (5.15 gm. Tl+ per 100 gm. triglycine sulfate in solution). A study was made of the effect of all the monovalent alkali metal ions Li Na' K Rb+ and Cs+ using the same concentration in each case (1 gm.-atom alkali-metal ion per 6.13 gm.-mols triglycine sulfate in solution). The enhanced [101] effect on triglycine sulfate increases as the ionic radius of the ion increases. Li+ has very little effect even at concentrations as high as 3 gm.-atms Li+ per 6.13 grn=rnols triglycine sulfate in solution. R-b Cs+ and Tl" each give the maximum effect. Other monovalent cations included in the study were NHJ, N(CH and Ag+. Approximately twice the concentration of NHJ or N(CH is required to enhance the [101] faces to approximately the same degree as K Ag+ present to the saturation point for Ag SO in the triglycine sulfate solution at 46 C. causes a very small enhancement of the [101] faces. Several other positive ions were studied in regard to their effect on triglycine sulfate crystal habit. Those studied include Cu++, Cd+ VO UO In+++ and Er+++. None of these ions exhibited any effect similar to that caused by the monovalent ions re ported above. Cd++, Er+++ and In+++ show practically no effect on triglycine sulfate crystal habit. Cu++, V0- and U0 show appreciable influence on triglycine sulfate crystal habit, but the results are yet to be correlated.
In growing the modified habit triglycine sulfate crystals, a small seed crystal having the desired thickness is drilled and mounted on a glass rod so that the [101] faces of the crystal are perpendicular to the rod. The seed is then planted in a glass container containing approximately 1400 ml. of saturated solution containing the required impurity addition at a temperature of 0.1 to 1.0 C. above the saturation temperature. The glass container is immersed in a water bath controlled to i0.02 C. by means of a magnetic set, mercury thermoregulator and a sensitive electronic relay. The temperature is programmed down at rates varying from 02 C. to 0.5 C. per day until the crystal reaches the desired size. Agitation within the solution is achieved by means of a magnetic stirrer.
It is believed that this habit described above should apply as well to the ferroelectric compounds of triglycine selenate, triglycine fluoberylate, and other similar compounds that are isomorphous to triglycine sulfate.
Changes in crystal habit are generally brought about by changes inone or more of the following factors:
(1) pH of the solution (2) Rate of growth (3) Interaction between solute and solvent (crystal habit may be changed depending on solvent used) (4) Concentration of growth active impurities a. Organic dyes b. Inorganic cations and anions Since the majority of laboratory controlled crystal habit modifications reported in publications fall under item (4) above, this approach was attempted as well in subsidiary investigations of triglycine sulfate. Several organic dyes were used as impurity additions to saturated triglycine sulfate solutions in concentrations on a weight basis ranging from 1 part dye: 8000 parts triglycine sulfate to 1 part dye: 1000 parts triglycine sulfate. The dyes used included Niagara Sky Blue BB,v Buffalo Black NBR, Trypan Red, Congo Red and Brilliant Cresyl Blue. Only minor habit modifications were obtained with any of the above dyes, and none were of practical application. Mechanical methods of inhibiting growth could be employed, such as placing the seed between glass plates, but this would conceivably lead to serious problems in obtaining uniform growth because of the difficulty of circulating the solution uniformly about the seed.
This invention, the controlled habit modification of triglycine sulfate and deuterated triglycine sulfate by means of monovalent cations, has resulted in low dispersion of the ferroelectric axis in single crystal plates thus grown and has permitted the fabrication of uniform thin sections from these plates, in turn permit-ting the building of ferroelectric devices with greater uniformity of electrical properties and simplicity of fabrication and construction.
Obviously many modifications and variations of the present invention are possible in the light of the above teachings. It is therefore to be understood that within the scope of the appended claims the invention may be practiced otherwise than as specifically described.
What is claimed is:
1. A method for habit modification and preparation of relatively large but thin single crystal plates of triglycine sulfate and deuterated triglycine sulfate having highly desirable crystal habit for use in ferroelectric devices, comprising:
(a) cutting a seed crystal of triglycine such that the distance between the (101) faces of the crystal determines the thickness of the crystal to be grown,
(b) planting said seed crystal in a suitably agitated saturated triglycine sulfate solution containing at least one impurity for preventing growth in the crystallographic [001] direction chosen from Rb CS and Tl+ ions,
(c) programming the temperature of said saturated solution downward for a suitable period of time consistent with crystal growth until the crystal grows to the desired size substantially only in two dimensions with substantially no growth in the crystallographic [001] direction.
ZJThe method for habit modification and preparation of relatively large but thin single crystal plates of tri- 30 glycine sulfate and deuterated triglycine sulfate having highly desirable crystal habit, comprising:
(a) mounting a seed crystalof triglycine on a support rod such that the rod extends from one of the (101) faces of the crystal, the desired thickness of the crystal to be grown being determined by the distance between the (101) faces of the seed crystal used,
(b) planting said seed crystal in a saturated triglycine sulfate solution containing Tl+ ions as an impurity for effectively preventing crystal growth inthe crystallographic [001] direction in a concentration in excess of 1 gm.-atom '1'l+:l235 gm.-mols triglycine sulfate in solution,
(c) programming the temperature of said saturated solution downward from the saturation temperature at suitable varying rates per day and with minimum fluctuation of temperature consistent with the growth of a single crystal until the crystal grows only in two dimensions to the desired size,
ing the period of crystal growth, resulting in uniform growth of crystal plates substantially only in two dimensions with substantially no growth in the crystallographic [001] direction to produce thin single crystal plates whose ferroelectric axis lies in the plane of the crystal plate and its direction within the plate has a much smaller dispersion than crystals of the same material having the normal habit.
3. The method for habit modification and prepara- 0 tion of relatively large but thin single crystal plates of triglycine sulfate and deuterated triglycine sulfate having highly desirable crystal habit, comprising:
(a) mounting a seed crystal of triglycine on a support rod such that the rod extends from one of the (101) faces of the crystal, the desired thickness of the crystal to be grown beingdetermined by the distance between the (101) faces of the seed crystal used,
(b) planting said seed crystal in a saturated triglycine sulfate solution containing Rb+ ions as an impurity for effectively preventing crystal growth in the crystallographic [001] direction,
(c) programming the temperautre of said saturated solution downward from the saturation temperature at suitable varying rates per day and with minimum fluctuation of temperature consistent with the growth (d) and agitating said solution by suitable means dur-' of a single crystal until the crystal grows only in two dimensions to the desired size,
((1) and agitating said solution by suitable means during the period of crystal growth, resulting in uniform growth of crystal plates substantially only in two dimensions with substantially no growth in the crystallographic [001] direction to produce thin single crystal plates whose ferroelectric axis lies in the plane of the crystal plate and its direction within the plate has a much smaller dispersion than crystals of the same material having the normal habit.
4. The method for habit modification and preparation of relatively large but thin single crystal plates of triglycine sulfate and deuterated triglycine sulfate having highly desirable crystal habit, comprising:
(a) mounting a seed crystal of triglycine on a support rod such that the rod extends from one of the (101) faces of the crystal, the desired thickness of the crystal to be grown being determined by the thickness of the seed crystal used,
(b) planting said seed crystal in a saturated triglycine sulfate solution containing Cs+ ions as an impurity for effectively preventing crystal growth in the crystallographic [001] direction,
(c) programming the temperature of said saturated solution downward from the saturation temperature at suitable varying rates per day and with minimum fluctuation of temperature consistent with the growth of a single crystal until the crystal grows only in two dimensions to the desired size,
(d) and agitating said solution by suitable means during the period of crystal growth, resulting in uniform growth of crystal plates substantially only in two dimensions with substantially no growth in the crystallographic [001] direction to produce thin single crystal plates whose ferro-electric axis lies in the plane of the crystal plate and its direction within the plate has a much smaller dispersion than crystals of the same material having the normal habit.
References Cited UNITED STATES PATENTS 5/1961 Matthias 260534 X
Claims (1)
1. A METHOD FOR HABIT MODIFICATION AND PREPARATION OF RELATIVELY LARGE BUT THIN SINGLE CRYSTAL PLATES OF TRIGLYCINE SULFATE AND DEUTERATED TRIGLYCINE SULFATE HAVING HIGHLY DESIRABLE CRYSTAL HABIT FOR USE IN FERROELECTRIC DEVICES, COMPRISING: (A) CUTTING A SEED CRYSTAL OF TRIGLYCINE SUCH THAT THE DISTANCE BETWEEN THE (101) FACES OF THE CRYSTAL DETERMINES THE THICKNESS OF THE CRYSTAL TO BE GROWN, (B) PLANTING SAID SEED CRYSTAL IN A SUITABLY AGITATED SATURATED TRIGLYCINE SULFATE SOLUTION CONTAINING AT LEAST ONE IMPURITY FOR PREVENTING GROWTH IN THE CRYSTALLOGRAPHIC (001) DIRECTION CHOSEN FROM RB+, CS+, AND T1+ IONS, (C) PROGRAMMING THE TEMPERATURE OF SAID SATURATED SOLUTION DOWNWARD FOR A SUITABLE PERIOD OF TIME CONSISTENT WITH CRYSTAL GROWTH UNTIL THE CRYSTAL GROWS TO THE DESIRED SIZE SUBSTANTIALLY ONLY IN TWO DIMENSIONS WITH SUBSTANTIALLY NO GROWTH IN THE CRYSTALLOGRAPHIC (100) DIRECTION.
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| US256175A US3352906A (en) | 1963-02-04 | 1963-02-04 | Habit modification and preparation of single crystal triglycine sulfate |
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| US256175A US3352906A (en) | 1963-02-04 | 1963-02-04 | Habit modification and preparation of single crystal triglycine sulfate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3953503A (en) * | 1968-02-21 | 1976-04-27 | Hitachi, Ltd. | Method of manufacturing triglycine series ferroelectric crystals |
| US4648991A (en) * | 1984-05-30 | 1987-03-10 | Research Corporation | Pyroelectric crystals with high figures of merit |
| US20060122265A1 (en) * | 2003-01-20 | 2006-06-08 | Sabine Pfeffer | Process for modifying drug crystal formation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2986681A (en) * | 1956-10-31 | 1961-05-30 | Bell Telephone Labor Inc | Monoclinic glycine sulfate and isomorphs |
-
1963
- 1963-02-04 US US256175A patent/US3352906A/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2986681A (en) * | 1956-10-31 | 1961-05-30 | Bell Telephone Labor Inc | Monoclinic glycine sulfate and isomorphs |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3953503A (en) * | 1968-02-21 | 1976-04-27 | Hitachi, Ltd. | Method of manufacturing triglycine series ferroelectric crystals |
| US4648991A (en) * | 1984-05-30 | 1987-03-10 | Research Corporation | Pyroelectric crystals with high figures of merit |
| US20060122265A1 (en) * | 2003-01-20 | 2006-06-08 | Sabine Pfeffer | Process for modifying drug crystal formation |
| US20090209639A1 (en) * | 2003-01-20 | 2009-08-20 | Sabine Pfeffer | Process for modifying drug crystal formation |
| US8008511B2 (en) | 2003-01-20 | 2011-08-30 | Novartis Ag | Process for modifying drug crystal formation |
| US8124795B2 (en) | 2003-01-20 | 2012-02-28 | Novartis Ag | Process for modifying drug crystal formation |
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