CN113769658A - Method for manufacturing novel heating body for synthesizing polycrystalline diamond - Google Patents
Method for manufacturing novel heating body for synthesizing polycrystalline diamond Download PDFInfo
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- CN113769658A CN113769658A CN202111138807.8A CN202111138807A CN113769658A CN 113769658 A CN113769658 A CN 113769658A CN 202111138807 A CN202111138807 A CN 202111138807A CN 113769658 A CN113769658 A CN 113769658A
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- polycrystalline diamond
- heating body
- synthesizing
- novel heating
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 50
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 27
- 239000010432 diamond Substances 0.000 title claims abstract description 27
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 62
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 13
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 238000005554 pickling Methods 0.000 claims abstract description 4
- 238000000746 purification Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims description 42
- 239000003513 alkali Substances 0.000 claims description 18
- 238000003723 Smelting Methods 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005242 forging Methods 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 18
- 238000003860 storage Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- 229910020968 MoSi2 Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000004568 cement Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910016006 MoSi Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/26—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Ceramic Products (AREA)
Abstract
The invention provides a method for manufacturing a novel heating body for synthesizing polycrystalline diamond. The manufacturing method of the novel heating body for synthesizing the polycrystalline diamond comprises the following steps: s1, selecting raw materials: (1) selecting: SiC (silicon carbide); s2, purification: (1) placing the SiC raw material selected in the first step into a container added with sulfuric acid, and heating and pickling to remove impurities such as metallic iron, iron oxide and the like on the surface of SiC. According to the manufacturing method of the novel heating body for synthesizing the polycrystalline diamond, provided by the invention, the SiC is used as the novel heating body, so that the novel heating body can continuously keep a stable temperature field under an ultrahigh pressure condition, the storage capacity is rich, the cost is lower, and the synthetic requirement of a superhard material can be greatly met.
Description
Technical Field
The invention belongs to the technical field of preparation of raw and auxiliary materials for high-pressure synthesis of superhard materials, and particularly relates to a manufacturing method of a novel heating body for synthesizing polycrystalline diamond.
Background
The large-scale polycrystalline diamond is formed by directly converting non-diamond carbon substances under the condition of ultrahigh pressure and high temperature, and the related technology discloses a heating sheet for synthesizing the polycrystalline diamond and a preparation method thereof. 1) Manufacturing an outer ring plate, grinding 80-90 parts of dolomite into powder, adding 10-15 parts of glass cement, uniformly stirring, and pressing into a wafer with the thickness of 3mm and the diameter of 4 cm; 2) manufacturing an inner ring sheet, grinding 20-30 parts of mica and 40-50 parts of graphite powder, uniformly mixing, adding 1-5 parts of glass cement, uniformly stirring, and pressing into a wafer with the thickness of 1mm and the diameter of 3 cm; 3) and (4) pressing and forming, namely placing the inner ring piece in the center of the outer ring piece, and flattening the inner ring piece and the outer ring piece. Compared with the prior art, the heating plate can improve the per unit yield of the polycrystalline diamond by 20-30%. .
However, the above-described structure has disadvantages in that polycrystalline diamond is formed by direct conversion of non-diamond carbon material under the conditions of ultra-high pressure and high temperature, under which a stable temperature field cannot be continuously generated by the heating material used, and graphite is converted into diamond to become an insulator under the conditions, and a common high temperature resistant metal cannot reach such a high temperature, so that only a noble metal such as rhenium (Re) can be used, but this method is expensive.
Therefore, there is a need to provide a new method for manufacturing a novel heater for synthesizing polycrystalline diamond to solve the above-mentioned problems.
Disclosure of Invention
The invention aims to provide a method for manufacturing a novel heating body for synthesizing polycrystalline diamond, which can continuously keep a stable temperature field under an ultrahigh pressure condition by adopting SiC as the novel heating body, has rich reserves and lower cost, and can greatly meet the synthesis requirement of superhard materials.
In order to solve the technical problem, the manufacturing method of the novel heating body for synthesizing the polycrystalline diamond, provided by the invention, comprises the following steps of:
s1, selecting raw materials:
(1) selecting: SiC (silicon carbide);
s2, purification:
(1) placing the SiC raw material selected in the first step into a container added with sulfuric acid, and heating and pickling to remove impurities such as metallic iron, ferric oxide and the like on the surface of SiC;
(2) cleaning the product after acid washing for 3-6min by using clean water, then placing the product into a container added with NAOH, and carrying out alkali washing to remove impurities such as free silicon, silicon dioxide and the like on the surface of SiC, thereby improving the content of silicon carbide;
(3) washing the product after alkali washing with clean water for 3-6min, and drying to obtain purified SiC.
As a further scheme of the invention, the acid washing time in the step (2) is 10-30min, and the temperature is 50-80 ℃.
As a further scheme of the invention, the alkali washing time in the step (3) is 10-20min, and the temperature is 40-60 ℃.
As a further aspect of the present invention, the method further includes S2:
(1) putting the obtained purified SiC into a smelting furnace for smelting to obtain a blank;
(2) forging and turning the obtained blank into a tubular shape or a sheet shape;
(3) and placing the processed tubular article or sheet article into a sintering and quenching integrated furnace to perform hydrogen atmosphere sintering for 1-3h, and further obtaining the required heating pipe or heating sheet.
As a further scheme of the invention, the smelting temperature of the first step in S2 is 1700C-2200 ℃ and the time is 30-120 min.
Compared with the prior art, the manufacturing method of the novel heating body for synthesizing the polycrystalline diamond has the following beneficial effects:
1. the invention adopts SiC as a novel heating body, so that the novel heating body can continuously maintain a stable temperature field under the condition of ultrahigh pressure, and has rich reserves and lower cost, thereby greatly meeting the synthesis requirement of superhard materials.
Detailed Description
The manufacturing method of the novel heating body for synthesizing the polycrystalline diamond comprises the following steps:
s1, selecting raw materials:
(1) selecting: SiC (silicon carbide);
s2, purification:
(1) placing the SiC raw material selected in the first step into a container added with sulfuric acid, and heating and pickling to remove impurities such as metallic iron, ferric oxide and the like on the surface of SiC;
(2) cleaning the product after acid washing for 3-6min by using clean water, then placing the product into a container added with NAOH, and carrying out alkali washing to remove impurities such as free silicon, silicon dioxide and the like on the surface of SiC, thereby improving the content of silicon carbide;
(3) washing the product after alkali washing with clean water for 3-6min, and drying to obtain purified SiC.
The acid washing time in the step (2) is 10-30min, and the temperature is 50-80 ℃.
The alkali washing time in the step (3) is 10-20min, and the temperature is 40-60 ℃.
Further comprises S2, forming:
(1) putting the obtained purified SiC into a smelting furnace for smelting to obtain a blank;
(2) forging and turning the obtained blank into a tubular shape or a sheet shape;
(3) and placing the processed tubular article or sheet article into a sintering and quenching integrated furnace to perform hydrogen atmosphere sintering for 1-3h, and further obtaining the required heating pipe or heating sheet.
The smelting temperature of the first step in the S2 is 1700C-2200 ℃, and the time is 30-120 min.
The principle of the manufacturing method of the novel heating body for synthesizing the polycrystalline diamond provided by the invention is as follows:
the first step is as follows: by adopting SiC as a novel heating body, the temperature field can be continuously kept stable under the condition of ultrahigh pressure, the storage capacity is rich, the cost is low, and the synthesis requirement of the superhard material can be greatly met.
In addition to the above mentioned method, MoSi2 material can be used, proper MoSi2 bar material is selected, the required heating tube or heating sheet can be obtained by turning, and the method of compounding metal (iron, tantalum) and SiC or MoSi2 material can be used, that is, the inside or outside of SiC or MoSi2 material is wrapped by metal, the metal is heated at low temperature, after reaching a certain temperature, the SiC or MoSi2 material starts to heat, so as to reach the effect of heating body, and MoSi2 material or the MoSi 3538 material and the metal are compounded to be used as a novel heating body, so that the stable temperature field can be continuously maintained under the condition of ultrahigh pressure, the reserves are abundant, the cost is low, and the synthesis requirement of superhard material can be greatly met.
Example 1:
the manufacturing method of the novel heating body for synthesizing the polycrystalline diamond comprises the following steps:
(1) selecting: SiC (silicon carbide);
(2) placing the SiC raw material selected in the first step into a container added with sulfuric acid, and carrying out heating and acid washing to remove impurities such as metallic iron, iron oxide and the like on the surface of SiC, wherein the acid washing time is 30min and the temperature is 50 ℃;
(3) washing the product after acid washing for 6min by clear water, then placing the product into a container added with NAOH, and carrying out alkali washing to remove impurities such as free silicon, silicon dioxide and the like on the surface of SiC, thereby improving the content of silicon carbide, wherein the alkali washing time is 20min, and the temperature is 40 ℃;
(4) washing the product after alkali washing with clean water for 6min, and then drying to obtain purified SiC;
(5) smelting the obtained purified SiC in a smelting furnace to obtain a blank, wherein the smelting temperature is 2200 ℃ and the time is 30 min;
(6) forging and turning the obtained blank into a tubular shape or a sheet shape;
(7) placing the processed tubular article or sheet article into a sintering and quenching integrated furnace to perform hydrogen atmosphere sintering for 3 hours to obtain a required heating pipe or heating sheet;
by adopting SiC as a novel heating body, the temperature field can be continuously kept stable under the condition of ultrahigh pressure, the storage capacity is rich, the cost is low, and the synthesis requirement of the superhard material can be greatly met.
Example 2:
the manufacturing method of the novel heating body for synthesizing the polycrystalline diamond comprises the following steps:
(1) selecting: SiC (silicon carbide);
(2) placing the SiC raw material selected in the first step into a container added with sulfuric acid, and carrying out heating and acid washing to remove impurities such as metallic iron, iron oxide and the like on the surface of SiC, wherein the acid washing time is 20min and the temperature is 65 ℃;
(3) washing the product after acid washing with clear water for 4.5min, then placing the product into a container with added NAOH, and carrying out alkali washing to remove impurities such as free silicon, silicon dioxide and the like on the surface of SiC, thereby improving the content of silicon carbide, wherein the alkali washing time is 15min and the temperature is 50 ℃;
(4) washing the product after alkali washing with clear water for 4.5min, and then drying to obtain purified SiC;
(5) smelting the obtained purified SiC in a smelting furnace at 1950 ℃ for 70min to obtain a blank;
(6) forging and turning the obtained blank into a tubular shape or a sheet shape;
(7) placing the processed tubular article or sheet article into a sintering and quenching integrated furnace to perform hydrogen atmosphere sintering for 2 hours to obtain a required heating pipe or heating sheet;
by adopting SiC as a novel heating body, the temperature field can be continuously kept stable under the condition of ultrahigh pressure, the storage capacity is rich, the cost is low, and the synthesis requirement of the superhard material can be greatly met.
Example 3:
the manufacturing method of the novel heating body for synthesizing the polycrystalline diamond comprises the following steps:
(1) selecting: SiC (silicon carbide);
(2) placing the SiC raw material selected in the first step into a container added with sulfuric acid, and carrying out heating and acid washing to remove impurities such as metallic iron, iron oxide and the like on the surface of SiC, wherein the acid washing time is 10min and the temperature is 80 ℃;
(3) washing the product after acid washing for 3min by clear water, then placing the product into a container added with NAOH, and carrying out alkali washing to remove impurities such as free silicon, silicon dioxide and the like on the surface of SiC, thereby improving the content of silicon carbide, wherein the alkali washing time is 10min, and the temperature is 60 ℃;
(4) washing the product after alkali washing with clear water for 3min, and then drying to obtain purified SiC;
(5) smelting the obtained purified SiC in a smelting furnace to obtain a blank, wherein the smelting temperature is 1700 ℃, and the time is 120 min;
(6) forging and turning the obtained blank into a tubular shape or a sheet shape;
(7) placing the processed tubular article or sheet article into a sintering and quenching integrated furnace to perform hydrogen atmosphere sintering for 1h to obtain a required heating pipe or heating sheet;
by adopting SiC as a novel heating body, the temperature field can be continuously kept stable under the condition of ultrahigh pressure, the storage capacity is rich, the cost is low, and the synthesis requirement of the superhard material can be greatly met.
Claims (5)
1. A method for manufacturing a novel heating body for synthesizing polycrystalline diamond is characterized by comprising the following steps:
s1, selecting raw materials:
(1) selecting: SiC (silicon carbide);
s2, purification:
(1) placing the SiC raw material selected in the first step into a container added with sulfuric acid, and heating and pickling to remove impurities such as metallic iron, ferric oxide and the like on the surface of SiC;
(2) cleaning the product after acid washing for 3-6min by using clean water, then placing the product into a container added with NAOH, and carrying out alkali washing to remove impurities such as free silicon, silicon dioxide and the like on the surface of SiC, thereby improving the content of silicon carbide;
(3) washing the product after alkali washing with clean water for 3-6min, and drying to obtain purified SiC.
2. The method of producing a novel heater for synthesizing polycrystalline diamond according to claim 1, wherein: the acid washing time in the step (2) is 10-30min, and the temperature is 50-80 ℃.
3. The method of producing a novel heater for synthesizing polycrystalline diamond according to claim 1, wherein: the alkali washing time in the step (3) is 10-20min, and the temperature is 40-60 ℃.
4. The method of producing a novel heater for synthesizing polycrystalline diamond according to claim 1, wherein: further comprises S2, forming:
(1) putting the obtained purified SiC into a smelting furnace for smelting to obtain a blank;
(2) forging and turning the obtained blank into a tubular shape or a sheet shape;
(3) and placing the processed tubular article or sheet article into a sintering and quenching integrated furnace to perform hydrogen atmosphere sintering for 1-3h, and further obtaining the required heating pipe or heating sheet.
5. The method of producing a novel heater for synthesizing polycrystalline diamond according to claim 4, wherein: the smelting temperature of the first step in the S2 is 1700C-2200 ℃, and the time is 30-120 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111138807.8A CN113769658A (en) | 2021-09-27 | 2021-09-27 | Method for manufacturing novel heating body for synthesizing polycrystalline diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111138807.8A CN113769658A (en) | 2021-09-27 | 2021-09-27 | Method for manufacturing novel heating body for synthesizing polycrystalline diamond |
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| Publication Number | Publication Date |
|---|---|
| CN113769658A true CN113769658A (en) | 2021-12-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111138807.8A Pending CN113769658A (en) | 2021-09-27 | 2021-09-27 | Method for manufacturing novel heating body for synthesizing polycrystalline diamond |
Country Status (1)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320602A (en) * | 2011-08-18 | 2012-01-18 | 白山峰泰源研磨材有限公司 | Purifying method of green silicon-carbide micropowder |
| CN104646928A (en) * | 2013-11-21 | 2015-05-27 | 蔡立超 | Manufacturing method of heating pipe of heating element of composite diamond |
-
2021
- 2021-09-27 CN CN202111138807.8A patent/CN113769658A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320602A (en) * | 2011-08-18 | 2012-01-18 | 白山峰泰源研磨材有限公司 | Purifying method of green silicon-carbide micropowder |
| CN104646928A (en) * | 2013-11-21 | 2015-05-27 | 蔡立超 | Manufacturing method of heating pipe of heating element of composite diamond |
Non-Patent Citations (1)
| Title |
|---|
| 龚汨清: "碳化硅加热元件的电性能和使用", 《微细加工技术》, no. 2, pages 71 - 78 * |
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