CN113860855A - Method for manufacturing pressure transmission medium used in ultrahigh pressure environment - Google Patents
Method for manufacturing pressure transmission medium used in ultrahigh pressure environment Download PDFInfo
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- C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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Abstract
The invention provides a method for manufacturing a pressure transmission medium used in an ultrahigh pressure environment. The manufacturing method of the pressure transmission medium used in the ultrahigh pressure environment comprises the following steps: s1, selecting raw materials: (1) selecting raw materials: MgO (magnesium oxide) and TiO2(titanium dioxide), CoO (cobalt oxide), Cr2O3(chromium oxide), Fe2O3(iron sesquioxide). The method for preparing the pressure transmission medium used in the ultrahigh-pressure environment adopts magnesium oxide doped with titanium dioxide, cobalt oxide, chromium oxide, ferric oxide and the like as a novel pressure transmission medium, has no phase change under the conditions of high pressure and high temperature, does not decompose substances which are easy to cause blasting, such as water, gas and the like, and is doped with the substancesThe heat conductivity of the cobalt oxide, the chromium oxide, the ferric oxide and other substances is reduced to a certain extent, and the reserves are rich, so that the synthesis requirement of the superhard material can be greatly met.
Description
Technical Field
The invention belongs to the technical field of superhard material raw and auxiliary material preparation, and particularly relates to a method for manufacturing a pressure transmission medium used in an ultrahigh pressure environment.
Background
Large-scale polycrystalline diamond is formed by direct conversion of non-diamond carbon species at ultra-high pressures and temperatures. Under the condition, pyrophyllite pressure transmission medium cannot meet the requirement of synthesizing polycrystalline diamond, so magnesium oxide is generally adopted as the pressure transmission medium under the condition at present, and in the related technology, a method for preparing polycrystalline diamond microspheres by hydro-thermal synthesis of carbon spheres is disclosed, and belongs to the field of material preparation. The method takes 0.1-0.2 mol/L glucose solution as raw material, and utilizes a hydrothermal method to synthesize carbon microspheres in a 200 ℃ oven for 24 hours at constant temperature; the prepared carbon microspheres are dispersed into sodium chloride superfine powder obtained by ball milling to form a mixture which is used as a raw material, the mixture is put into a mould for compression molding, the mixture is put into a magnesium oxide crucible after demoulding, and the magnesium oxide, a rhenium tube furnace, a lanthanum chromate ring and an aluminum oxide column which are used as pressure transfer media form an assembly block, and the assembly block is put into an oven to be kept at the constant temperature of 120 ℃ for 3 to 4 hours; and taking out the assembly block, placing the assembly block in a high-temperature and high-pressure device, and reacting at high temperature under ultrahigh pressure to obtain the polycrystalline diamond microspheres. The polycrystalline diamond microspheres prepared by the method do not contain any catalyst, and the obtained diamond microspheres have uniform size and compact blocks, and the Vickers hardness reaches 60-80 GPa.
However, the above structure has disadvantages because the pressure transmission medium is magnesium oxide, which has high thermal conductivity and needs to be added with heat insulation pipes in the cavity, thus reducing the effective cavity.
Therefore, it is necessary to provide a new method for manufacturing a pressure transmission medium used in an ultra-high pressure environment to solve the above-mentioned technical problems.
Disclosure of Invention
The invention aims to provide a method for preparing a pressure transmission medium used in an ultrahigh pressure environment, which adopts magnesium oxide doped with titanium dioxide, cobalt oxide, chromium oxide, ferric oxide and the like as a novel pressure transmission medium, has no phase change under the conditions of high pressure and high temperature, does not decompose substances which easily cause blasting such as water, gas and the like, and has certain reduction of the thermal conductivity of the magnesium oxide and abundant reserves, thereby greatly meeting the synthesis requirement of superhard materials.
In order to solve the technical problem, the method for manufacturing the pressure transmission medium used in the ultrahigh pressure environment comprises the following steps:
s1, selecting raw materials:
(1) selecting raw materials: MgO (magnesium oxide) and TiO2(titanium dioxide), CoO (cobalt oxide), Cr2O3(chromium oxide), Fe2O3(iron sesquioxide);
s2, a manufacturing process:
(1) mixing the above materials at a certain ratio2、CoO、Cr2O3、Fe2O3One or more raw materials are put into a ball mill, alcohol with a certain proportion is added, so that the raw materials can be fully and uniformly mixed for 2-4 h;
(2) drying the product obtained by mixing through drying equipment for 3-5 min;
(3) placing the product obtained in the step (2) into crushing equipment for crushing for 20-40 min;
(4) placing the crushed product obtained in the step (3) on a press machine for press forming.
As a further scheme of the invention, the pressure of the press is 4-12MPa, and the time is 10-20 min.
As a further scheme of the invention, the proportion of MgO is 60-90%, and TiO is2、CoO、Cr2O3、Fe2O3The proportion of (A) is 40-10%.
As a further aspect of the present invention, the method further includes S3:
(1) and (3) placing the formed product obtained in the step (4) into a muffle furnace for high-temperature sintering, and further obtaining the required pressure transmission medium.
As a further scheme of the invention, the temperature in the muffle furnace in the step S3 is 1300-1600 ℃, and the time is 30-120 min.
Compared with the related technology, the method for manufacturing the pressure transmission medium used in the ultrahigh pressure environment has the following beneficial effects:
the invention adopts magnesium oxide doped with titanium dioxide, cobalt oxide, chromium oxide, ferric oxide and the like as novel pressure transmission media, has no phase change under the conditions of high pressure and high temperature, does not decompose substances which are easy to cause blasting such as water, gas and the like, and the doped substances such as cobalt oxide, chromium oxide, ferric oxide and the like are substances which can reduce the thermal conductivity of magnesium oxide to a certain extent and have rich reserves, thereby greatly meeting the synthesis requirement of superhard materials and being used under the condition of ultrahigh pressure of more than 10 GPa.
Detailed Description
The manufacturing method of the pressure transmission medium used in the ultrahigh pressure environment comprises the following steps:
s1, selecting raw materials:
(1) selecting raw materials: MgO (magnesium oxide) and TiO2(titanium dioxide), CoO (cobalt oxide), Cr2O3(chromium oxide), Fe2O3(iron sesquioxide);
s2, a manufacturing process:
(1) mixing the above materials at a certain ratio2、CoO、Cr2O3、Fe2O3One or more raw materials are put into a ball mill, alcohol with a certain proportion is added, so that the raw materials can be fully and uniformly mixed for 2-4 h;
(2) drying the product obtained by mixing through drying equipment for 3-5 min;
(3) placing the product obtained in the step (2) into crushing equipment for crushing for 20-40 min;
(4) placing the crushed product obtained in the step (3) on a press machine for press forming.
The pressure of the press is 4-12MPa, and the time is 10-20 min.
The proportion of MgO is 60-90%, and the TiO is2、CoO、Cr2O3、Fe2O3The proportion of (A) is 40-10%.
Further comprises S3, forming:
(1) and (3) placing the formed product obtained in the step (4) into a muffle furnace for high-temperature sintering, and further obtaining the required pressure transmission medium.
The temperature in the muffle furnace in the step S3 is 1300-1600 ℃, and the time is 30-120 min.
The principle of the method for manufacturing the pressure transmission medium used in the ultrahigh pressure environment is as follows:
because the magnesium oxide is doped with titanium dioxide, cobalt oxide, chromium oxide, ferric oxide and the like as novel pressure transmission media, the magnesium oxide has no phase change under the conditions of high pressure and high temperature, and does not decompose substances which are easy to cause blasting, such as water, gas and the like, the doped substances such as cobalt oxide, chromium oxide, ferric oxide and the like are substances which reduce the thermal conductivity of the magnesium oxide to a certain extent, and the reserves are rich, so that the synthetic requirement of superhard materials can be greatly met, and the magnesium oxide can be used under the condition of ultrahigh pressure of more than 10 GPa.
Example 1:
the manufacturing method of the pressure transmission medium used in the ultrahigh pressure environment comprises the following steps:
(1) selecting raw materials: MgO (magnesium oxide) and TiO2(titanium dioxide), CoO (cobalt oxide), Cr2O3(chromium oxide), Fe2O3(iron sesquioxide);
(2) mixing the above materials at a certain ratio2、CoO、Cr2O3、Fe2O3One or more raw materials are put into a ball mill, alcohol with a certain proportion is added, the raw materials can be fully and uniformly mixed for 4 hours, and the MgO is preparedThe proportion is 90 percent, the TiO2、CoO、Cr2O3、Fe2O3The proportion of (A) is 10%;
(3) drying the product obtained by mixing through drying equipment for 5 min;
(4) placing the product obtained in the step (2) into crushing equipment for crushing, wherein the crushing time is 40 min;
(5) placing the crushed product obtained in the step (3) on a press for press forming, wherein the pressure of the press is 12MPa, and the time is 20 min;
(6) and (3) placing the formed product obtained in the step (4) into a muffle furnace for high-temperature sintering to obtain the required pressure transmission medium, wherein the temperature in the muffle furnace in the step S3 is 1600 ℃ and the time is 120 min.
The principle is as follows: because the magnesium oxide is doped with titanium dioxide, cobalt oxide, chromium oxide, ferric oxide and the like as novel pressure transmission media, the magnesium oxide has no phase change under the conditions of high pressure and high temperature, and does not decompose substances which are easy to cause blasting, such as water, gas and the like, the doped substances such as cobalt oxide, chromium oxide, ferric oxide and the like are substances which reduce the thermal conductivity of the magnesium oxide to a certain extent, and the reserves are rich, so that the synthetic requirement of superhard materials can be greatly met, and the magnesium oxide can be used under the condition of ultrahigh pressure of more than 10 GPa.
Example 2:
the manufacturing method of the pressure transmission medium used in the ultrahigh pressure environment comprises the following steps:
(1) selecting raw materials: MgO (magnesium oxide) and TiO2(titanium dioxide), CoO (cobalt oxide), Cr2O3(chromium oxide), Fe2O3(iron sesquioxide);
(2) mixing the above materials at a certain ratio2、CoO、Cr2O3、Fe2O3One or more raw materials are put into a ball mill, alcohol with a certain proportion is added, the raw materials can be fully and uniformly mixed for 3 hours, the proportion of MgO is 75 percent, and TiO is added2、CoO、Cr2O3、Fe2O3The proportion of (A) is 25%;
(3) drying the product obtained by mixing through drying equipment for 3-5 min;
(4) placing the product obtained in the step (2) into crushing equipment for crushing for 30 min;
(5) placing the crushed product obtained in the step (3) on a press for pressing and forming, wherein the pressure of the press is 8MPa, and the time is 15 min;
(6) and (3) placing the formed product obtained in the step (4) into a muffle furnace for high-temperature sintering to obtain the required pressure transmission medium, wherein the temperature in the muffle furnace in the step S3 is 1450 ℃, and the time is 75 min.
The principle is as follows: because the magnesium oxide is doped with titanium dioxide, cobalt oxide, chromium oxide, ferric oxide and the like as novel pressure transmission media, the magnesium oxide has no phase change under the conditions of high pressure and high temperature, and does not decompose substances which are easy to cause blasting, such as water, gas and the like, the doped substances such as cobalt oxide, chromium oxide, ferric oxide and the like are substances which reduce the thermal conductivity of the magnesium oxide to a certain extent, and the reserves are rich, so that the synthetic requirement of superhard materials can be greatly met, and the magnesium oxide can be used under the condition of ultrahigh pressure of more than 10 GPa.
Example 3:
the manufacturing method of the pressure transmission medium used in the ultrahigh pressure environment comprises the following steps:
(1) selecting raw materials: MgO (magnesium oxide) and TiO2(titanium dioxide), CoO (cobalt oxide), Cr2O3(chromium oxide), Fe2O3(iron sesquioxide);
(2) mixing the above materials at a certain ratio2、CoO、Cr2O3、Fe2O3One or more raw materials are put into a ball mill, alcohol with a certain proportion is added, so that the raw materials can be fully and uniformly mixed for 2 hours, the proportion of MgO is 60 percent, and TiO is added2、CoO、Cr2O3、Fe2O3In a ratio of 40;
(3) drying the product obtained by mixing through drying equipment for 3 min;
(4) placing the product obtained in the step (2) into crushing equipment for crushing, wherein the crushing time is 20 min;
(5) placing the crushed product obtained in the step (3) on a press for press forming, wherein the pressure of the press is 4MPa, and the time is 10 min;
(6) and (3) placing the formed product obtained in the step (4) into a muffle furnace for high-temperature sintering to obtain the required pressure transmission medium, wherein the temperature in the muffle furnace in the step S3 is 1300 ℃, and the time is 30 min.
The principle is as follows: because the magnesium oxide is doped with titanium dioxide, cobalt oxide, chromium oxide, ferric oxide and the like as novel pressure transmission media, the magnesium oxide has no phase change under the conditions of high pressure and high temperature, and does not decompose substances which are easy to cause blasting, such as water, gas and the like, the doped substances such as cobalt oxide, chromium oxide, ferric oxide and the like are substances which reduce the thermal conductivity of the magnesium oxide to a certain extent, and the reserves are rich, so that the synthetic requirement of superhard materials can be greatly met, and the magnesium oxide can be used under the condition of ultrahigh pressure of more than 10 GPa.
Claims (5)
1. A method for manufacturing a pressure transmission medium used in an ultrahigh pressure environment is characterized by comprising the following steps:
s1, selecting raw materials:
(1) selecting raw materials: MgO (magnesium oxide) and TiO2(titanium dioxide), CoO (cobalt oxide), Cr2O3(chromium oxide), Fe2O3(iron sesquioxide);
s2, a manufacturing process:
(1) mixing the above materials at a certain ratio2、CoO、Cr2O3、Fe 2O3One or more raw materials are put into a ball mill, alcohol with a certain proportion is added, so that the raw materials can be fully and uniformly mixed for 2-4 h;
(2) drying the product obtained by mixing through drying equipment for 3-5 min;
(3) placing the product obtained in the step (2) into crushing equipment for crushing for 20-40 min;
(4) placing the crushed product obtained in the step (3) on a press machine for press forming.
2. The method for producing a pressure medium used in an ultrahigh-pressure environment according to claim 1, characterized in that: the pressure of the press is 4-12MPa, and the time is 10-20 min.
3. The method for producing a pressure medium used in an ultrahigh-pressure environment according to claim 1, characterized in that: the proportion of MgO is 60-90%, and the TiO is2、CoO、Cr2O3、Fe2O3The proportion of (A) is 40-10%.
4. The method for producing a pressure medium used in an ultrahigh-pressure environment according to claim 1, characterized in that: further comprises S3, forming:
(1) and (3) placing the formed product obtained in the step (4) into a muffle furnace for high-temperature sintering, and further obtaining the required pressure transmission medium.
5. The method for manufacturing a pressure medium used in an ultrahigh-pressure environment according to claim 4, wherein: the temperature in the muffle furnace in the step S3 is 1300-1600 ℃, and the time is 30-120 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114452896A (en) * | 2022-02-09 | 2022-05-10 | 南方科技大学 | Efficient pressure transmission assembly preparation method for ultrahigh-temperature and high-pressure experiment |
| CN115947612A (en) * | 2022-12-09 | 2023-04-11 | 秦皇岛琨煜晶材科技有限公司 | Pressure transmission medium for high temperature and high pressure |
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| CN111747731A (en) * | 2019-03-26 | 2020-10-09 | 中国科学院上海硅酸盐研究所 | Magnesium oxide based ultrahigh pressure dielectric ceramic and preparation method thereof |
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| CN115947612B (en) * | 2022-12-09 | 2023-09-12 | 秦皇岛琨煜晶材科技有限公司 | Pressure transmission medium for high temperature and high pressure |
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