Patent US3872222A successfully refreshed from Google Patents.
US3872222A
Expired / Lapsed
US
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Process for producing metal sulphide crystals
Assignee: Crysdyn Corp
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Filing: 1970-10-01
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Granted: 1975-03-18
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Expires: 1990-10-01
Abstract
Abstract Single isometric metal sulphide crystals suitable for use as semiconductors, phosphorus electroluminescents and radiation detectors and a method of forming them comprising crystallizing the metal sulphide from crystallizing solutions containing metal bisulphide complex ions, HS ions and an excess amount of metal sulphide ions, having a pH of 6-14.
Inventors
- 👤 Hubert L Barnes
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 17:55
CPC Classifications
C; C30; C30B; C30B7/00; C01; C01G; C01G1/00; C01G1/12; C30B29/00; C30B29/10; C30B29/46
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
180 words
A METHOD OF GROWING SINGLE ISOMETRIC METAL SULPHIDE CRYSTALS OF HIGH PURITY WHICH HAVE A DIMENSION OF 25 MICRONS OR MORE COMPRISING: A. FORMING A SATURATED AQUEOUS METAL SULPHIDE CRYSTALLIZING SOLUTION THAT HAS A PH OF 6 TO 14 AT A REFERENCE TEMPERATURE OF 25*C COMPRISING COMPOUNDS THAT FORM METAL BISULPHIDE COMPLEX IONS, HS- IONS, DISSOLVED H2S AND AN EXCESS AMOUNT OF METAL SULPHIDE NUTRIENT, IN WHICH (1) AT A PH ABOVE 7 THE HS- ION IS THE PREDOMINANT SULFUR CONTAINING ION IN SOLUTION AND (2) AT A PH BETWEEN 6 AND 7 CONTAINS DISSOLVED HYDROGEN SULPHIDE WHICH IS PREDOMINANT IN SOLUTION BUT THE HS- ION CONCENTRATION IS NOT LESS THAN 1/10TH OF THE H2S MOLAR CONCENTRATION IN THE SOLUTION, AND B. AFTER SAID CRYSTALLIZING SOLUTION REACHES A CHEMICAL EQUILIBRIUM BETWEEN SAID OETAL BISULPHIDE COMPLEX ION, SAID HS- AND SAID METAL SULPHIDE, SUBJECTING SAID CRYSTALLIZING SOLUTION TO A CHEMICAL POTENTIAL GRADIENT THAT CAUSES THE METAL BISULPHIDE COMPLEX ION TO DISSOCIATE TO FORM MORE METAL SULPHIDE WHICH INITIATES THE FORMATION AND THE GROWTH OF METAL SULPHIDE CRYSTALS IN THE CRYSTALLIZING SOLUTION.
Claim 2
Independent Claim
180 words
A METHOD OF GROWING SINGLE ISOMETRIC METAL SULPHIDE CRYSTALS OF HIGH PURITY WHICH HAVE A DIMENSION OF 25 MICRONS OR MORE COMPRISING: A. FORMING A SATURATED AQUEOUS METAL SULPHIDE CRYSTALLIZING SOLUTION THAT HAS A PH OF 6 TO 14 AT A REFERENCE TEMPERATURE OF 25*C COMPRISING COMPOUNDS THAT FORM METAL BISULPHIDE COMPLEX IONS, HS- IONS, DISSOLVED H2S AND AN EXCESS AMOUNT OF METAL SULPHIDE NUTRIENT, IN WHICH (1) AT A PH ABOVE 7 THE HS- ION IS THE PREDOMINANT SULFUR CONTAINING ION IN SOLUTION AND (2) AT A PH BETWEEN 6 AND 7 CONTAINS DISSOLVED HYDROGEN SULPHIDE WHICH IS PREDOMINANT IN SOLUTION BUT THE HS- ION CONCENTRATION IS NOT LESS THAN 1/10TH OF THE H2S MOLAR CONCENTRATION IN THE SOLUTION, AND B. AFTER SAID CRYSTALLIZING SOLUTION REACHES A CHEMICAL EQUILIBRIUM BETWEEN SAID OETAL BISULPHIDE COMPLEX ION, SAID HS- AND SAID METAL SULPHIDE, SUBJECTING SAID CRYSTALLIZING SOLUTION TO A CHEMICAL POTENTIAL GRADIENT THAT CAUSES THE METAL BISULPHIDE COMPLEX ION TO DISSOCIATE TO FORM MORE METAL SULPHIDE WHICH INITIATES THE FORMATION AND THE GROWTH OF METAL SULPHIDE CRYSTALS IN THE CRYSTALLIZING SOLUTION.
Claim 3
Dependent Claim
56 words
The method of claim 1, in which said metal bisulphide complex ions are formed by reacting a reactant selected from the group consisting of a metal and a metal salt in an aqueous solution of hydrogen sulphide and a compound selected from the group consisting of an alkali hydroxide, an alkali sulphide or an alkali bisulphide.
Claim 4
Dependent Claim
26 words
The method of claim 1, in which said metal sulphide nutrient is zinc sulphide and said metal bisulphide complex ion is a zinc bisulphide complex ion.
Claim 5
Dependent Claim
31 words
The method of claim 3, in which the solution is saturated with H2S, contains 6- 15 molal of the HS ions in solution and has a pH of 7.5 to 9.
Claim 6
Dependent Claim
17 words
The method of claim 4, in which the temperature is 350*-550*C and the temperature gradient is 10*-30*C.
Claim 7
Dependent Claim
40 words
The method of claim 1, in which said metal sulphide nutrient is a sulphide selected from the group consisting of V, Fe, Co, Ni, Cu, Zn, Ga, As, Mo, Cd, Ag, In, Sn, Sb, Au, Hg, Tl, Pb and Bi.
Claim 8
Dependent Claim
13 words
The process of claim 1, in which said chemical potential gradient is acidification.
Claim 9
Dependent Claim
12 words
The process of claim 1, in which said pH range is 7-9.
Claim 10
Dependent Claim
13 words
The process of claim 1, in which said pH range is above 9.
Claim 11
Dependent Claim
26 words
The process of claim 1, in which the temperature of the crystallizing solution is about 25*- 750*C and the pressure is about 1 to 1000 atmospheres.
Claim 12
Dependent Claim
32 words
The process of claim 1 in which the pH is adjusted so that the HS ion concentration exceeds 0.01 molal and the solubility of the metaL sulphide exceeds about 10 5 molal.
Claim 13
Dependent Claim
19 words
The process of claim 11 in which the concentration of the HS ion is approximately 5 to 10 molal.
Claim 14
Dependent Claim
25 words
The process of claim 1, in which the metal sulphide nutrient is HgS, the HS ion concentration is 4-15 molal and the pH is 7-9.
Claim 15
Dependent Claim
18 words
The process of claim 13, in which the temperature is 150*-250*C and the temperature gradient is 10*- 30*C.
Claim 16
Dependent Claim
26 words
The method of claim 1, in which said metal sulphide crystals are ZnS crystals, said metal sulphide nutrient is ZnS and said pH is 7- 9.
Claim 17
Dependent Claim
22 words
The method of claim 1, in which said metal sulphide crystals are mercury sulphide and said metal sulphide nutrient is mercury sulphide.
Claim 18
Dependent Claim
16 words
The process of claim 1, in which said chemical potential gradient is HS ion strength dilution.
Claim 19
Dependent Claim
14 words
The process of claim 1, in which said chemical potential gradient is pressure quenching.
Claim 20
Dependent Claim
13 words
The process of claim 1, in which said chemical potential gradient is oxidation.
Claim 21
Dependent Claim
14 words
The process of claim 1, in which said chemical potential gradient is temperature gradients.
References Cited (Backward Citations)
US3058807A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-03-17 | 1978-09-16 | 1979-03-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-03-17 | 1982-09-16 | 1983-03-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-03-17 | 1986-09-16 | 1987-03-18 | $7700.00 | Window Closed / Lapsed |