阅读说明：本技术 一种合成多晶金刚石用新型加热体的制作方法 (Method for manufacturing novel heating body for synthesizing polycrystalline diamond ) 是由 王永凯 张相法 位星 王大鹏 刘红伟 薛磊 赵帅 于 2021-09-27 设计创作，主要内容包括：本发明提供一种合成多晶金刚石用新型加热体的制作方法。所述合成多晶金刚石用新型加热体的制作方法包括以下步骤：S1、原材料选取：(1).选取：SiC(碳化硅)；S2、纯化：(1).将上述步骤一选取的SiC原料放置到加入硫酸的容器内,进行加热酸洗,使其去除SiC表面的金属铁和氧化铁等杂质。本发明提供的合成多晶金刚石用新型加热体的制作方法通过采用SiC作为新型加热体,使其能够在超高压条件下能够持续保持稳定的温度场,且其储量丰富,成本较低,从而可以极大的满足超硬材料合成要求的优点。(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.)

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.

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.