SU1490869A1 - Method of producing diamond powders - Google Patents
Method of producing diamond powders Download PDFInfo
- Publication number
- SU1490869A1 SU1490869A1 SU874310464A SU4310464A SU1490869A1 SU 1490869 A1 SU1490869 A1 SU 1490869A1 SU 874310464 A SU874310464 A SU 874310464A SU 4310464 A SU4310464 A SU 4310464A SU 1490869 A1 SU1490869 A1 SU 1490869A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- diamond
- potassium
- graphite
- argon
- content
- Prior art date
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- 239000010432 diamond Substances 0.000 title claims abstract description 21
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 12
- 239000011591 potassium Substances 0.000 claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 10
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011734 sodium Substances 0.000 claims abstract description 5
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 4
- 150000003624 transition metals Chemical class 0.000 claims abstract description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract 4
- 150000001340 alkali metals Chemical class 0.000 claims abstract 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract 3
- 238000001035 drying Methods 0.000 claims abstract 3
- 230000003647 oxidation Effects 0.000 claims abstract 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract 3
- 239000001301 oxygen Substances 0.000 claims abstract 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract 3
- 238000005406 washing Methods 0.000 claims abstract 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052742 iron Inorganic materials 0.000 abstract description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052744 lithium Inorganic materials 0.000 abstract description 4
- 229910052748 manganese Inorganic materials 0.000 abstract description 4
- 239000011572 manganese Substances 0.000 abstract description 4
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- -1 graphite compound Chemical class 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000035784 germination Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
Изобретение относитс к способам получени синтетических алмазов и может быть использовано в абразивной проьышленности. Цель - уменьшение примесей переходных металлов в порошках алмаза. Это достигаетс способом получени порошков алмаза при воздействии давлени и температуры в области стабильности алмаза на слоистое соединение графита с одним, или двум щелочными металлами, выбранными из группы,включающей литий, натрий, калий или их смеси, которые предварительно подвергают окислению кислородом воздуха или метанолом, или уксусной кислотой в среде аргона с последующей промывкой водой до остаточного содержани гцелочного металла 1 - 4 мас.% и сушкой до посто нной массы. Содержание примесей марганца не превышает 0,002 мас.%, железа 0,008 мас.% и никел 0,01 мас.%. слThe invention relates to methods for producing synthetic diamonds and can be used in the abrasive industry. The goal is to reduce the transition metal impurities in diamond powders. This is achieved by the method of obtaining diamond powders by applying pressure and temperature in the region of diamond stability to a layered graphite compound with one or two alkali metals selected from the group including lithium, sodium, potassium or their mixtures, which are previously subjected to oxidation with air oxygen or methanol, or with acetic acid in argon, followed by washing with water until 1 to 4 wt.% of the residual hectare metal and drying to constant weight. The content of manganese impurities does not exceed 0.002 wt.%, Iron 0.008 wt.% And nickel 0.01 wt.%. cl
Description
Изобретение относитс к с юсобам получени синтетических алмазов и может быть использовано в абразивной промышленности.The invention relates to the production of synthetic diamonds and can be used in the abrasive industry.
Целью изобретени вл етс уменьшение примесей переходных металлов в порошках алмазов.The aim of the invention is to reduce transition metal impurities in diamond powders.
Пример 1. К 20 г природного графита Завалевского месторождени в токе аргона при температуре порци ми прибавл ют 8,12 г кали , перемешивают 4 ч и получают слоистое соединение графита формулы , содержащее 29 мас.% кали . Затем в токе аргона его обрабатывают метанолом, отмывают водой до остаточного содержани кали 4 мас.Х и сушат при 150°СExample 1. 8.12 g of potassium is added in portions to 20 g of natural graphite of the Zavalevsky deposit in a stream of argon at a temperature, stirred for 4 hours to obtain a layered graphite compound of the formula containing 29% by weight of potassium. Then, in a stream of argon, it is treated with methanol, washed with water to a residual potassium content of 4% X. and dried at 150 ° С
до посто нной массы. Полученный порошок помещают в количестве 0,3 г в камеру высокого давлени типа тороид и воздействуют давлением 6 ГПа при 1300 С в течение 15 мин. Алмаз выде- л ют кип чением продуктА в хлорной кислоте. Выход алмаза составл ет 24 мас.%. Содержание примесей по данным масс-спектрометрического анализа составл ет, %: марганец 0,002; железо 0,008 и никель 0,01.to constant mass. The obtained powder is placed in an amount of 0.3 g in a toroid-type high-pressure chamber and is subjected to a pressure of 6 GPa at 1300 ° C for 15 minutes. Diamond was isolated by boiling the product A in perchloric acid. The diamond yield is 24% by weight. The content of impurities according to mass spectrometric analysis is,%: manganese 0.002; iron 0.008 and nickel 0.01.
Пример2..К10г графита в аргоне при 200 С добавл ют порци ми 0,96 г лити при перемешивании в течение 3 ч и получают слоистое соединение графита с литием CgLi. Кго окисл ют на воздухе при комнатной темпе-Example 2. K10g of graphite in argon at 200 ° C is added in portions of 0.96 g of lithium with stirring for 3 hours to obtain a layered compound of graphite with lithium CgLi. Cgo is oxidized in air at room temperature.
0000
ратуре, отмывают водой и сушат гг и ЮО С до посто нной массы. 0,15 г полученного соединени с содержанием 1,5 мас.Х лити помещают в камеру вы- сокого давлени и в течение 10 мин ведут синтез алмазов при давлении 12 П1а и температуре . Выход алмаза 35%. Содержание марганца 0,001%, железа 0,004% и хикел 0,006%. The mixture is washed with water and dried with yy and SO to constant weight. 0.15 g of the obtained compound with a content of 1.5% by weight of lithium is placed in a high-pressure chamber, and diamond synthesis is carried out for 10 minutes at a pressure of 12 μA and temperature. Diamond yield 35%. The content of manganese is 0.001%, iron is 0.004% and hickel is 0.006%.
ПримерЗ. К4г графита в токе аргона при перемешивании добавл ют 0,16 г натри и 1,0 г кали . За 3,5 ч получают слоистое соединение формулы С ,2 Na,o К. В токе аргона его об- рабатывают уксусной кислотой, отмывают водой и высушивают. 0,3 г продукта подвергают воздействию давлени 7,7 ГПа при температуре 1300°С в течении 3 мин. Выход алмаза 55 мае,7,. i Содержание примесей аналогично примеРУ 1 .Example K4g of graphite in a stream of argon added 0.16 g of sodium and 1.0 g of potassium with stirring. In 3.5 hours, a layered compound of the formula C, 2 Na, o K is obtained. In a stream of argon, it is treated with acetic acid, washed with water and dried. 0.3 g of the product is subjected to a pressure of 7.7 GPa at a temperature of 1300 ° C for 3 minutes. The output of the diamond is 55 May, 7 ,. i The content of impurities is similar to example 1.
П р и м е р 4. Соединение графита с калием, полученное по примеру 1, сPRI me R 4. The connection of graphite with potassium, obtained in example 1, with
вергают давлению 8 ГПа при 1450 С в течение 7 мин. После химической обработки получают 2,45 г алмаза. Выход алмаза 68 мас.%. Содержание марганца 0,001/J, железа 0,006% и никел 0,008%.They charge a pressure of 8 GPa at 1450 C for 7 minutes. After chemical treatment, 2.45 g of diamond is obtained. The output of the diamond 68 wt.%. The content of manganese is 0.001 / J, iron is 0.006% and nickel is 0.008%.
Полученные алмазы представл ют собой кристаллы октаздрической и ку- бооктаздрической формы, уплощенные шпинелевые двойники срастани и частичного прорастани с размером до 150 мкм. The diamonds obtained are octasdric and cuboctasdric crystals, flattened spinel twins of intergrowth and partial germination with a size of up to 150 microns.
Изобретение позвол ет получать алмазные порошки с высоким выходом и содержанием примесей переходных металлов - марганца, железа и никел - на пор док меньше (0,011-0,018), чем по способу-прототипу (0,17-0,22%).The invention makes it possible to produce diamond powders with a high yield and a content of impurities of transition metals — manganese, iron, and nickel — an order of magnitude less (0.011-0.018) than in the prototype method (0.17-0.22%).
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU874310464A SU1490869A1 (en) | 1987-09-30 | 1987-09-30 | Method of producing diamond powders |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU874310464A SU1490869A1 (en) | 1987-09-30 | 1987-09-30 | Method of producing diamond powders |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU1490869A1 true SU1490869A1 (en) | 1991-04-23 |
Family
ID=21329420
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU874310464A SU1490869A1 (en) | 1987-09-30 | 1987-09-30 | Method of producing diamond powders |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU1490869A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100430313C (en) * | 2006-01-20 | 2008-11-05 | 山东大学 | Controllable hydrothermal constant-pressure synthesis method for preparing boron-carbon-nitrogen material |
| CN100430314C (en) * | 2006-01-04 | 2008-11-05 | 山东大学 | Solvothermal constant-pressure synthesis method for regulating phase of boron-carbon-nitrogen material |
-
1987
- 1987-09-30 SU SU874310464A patent/SU1490869A1/en active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100430314C (en) * | 2006-01-04 | 2008-11-05 | 山东大学 | Solvothermal constant-pressure synthesis method for regulating phase of boron-carbon-nitrogen material |
| CN100430313C (en) * | 2006-01-20 | 2008-11-05 | 山东大学 | Controllable hydrothermal constant-pressure synthesis method for preparing boron-carbon-nitrogen material |
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