CN113816392A - Preparation method of hafnium boride powder - Google Patents
Preparation method of hafnium boride powder Download PDFInfo
- Publication number
- CN113816392A CN113816392A CN202111200190.8A CN202111200190A CN113816392A CN 113816392 A CN113816392 A CN 113816392A CN 202111200190 A CN202111200190 A CN 202111200190A CN 113816392 A CN113816392 A CN 113816392A
- Authority
- CN
- China
- Prior art keywords
- finished product
- powder
- semi
- preparation
- drying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
Abstract
The invention relates to a preparation method of hafnium boride powder, which can obtain the hafnium boride powder with high purity and ultra-fine granularity according to the operation flows of sequentially mixing, primarily grinding, primarily drying, vacuum synthesizing, crushing, primarily sieving, secondarily drying and secondarily sieving raw materials of hafnium oxide, boron carbide and carbon black. That is, the present invention can improve not only the purity of the prepared hafnium boride powder but also the fineness of the particle size of the prepared hafnium boride powder.
Description
Technical Field
The invention relates to the technical field of hafnium boride preparation, in particular to a preparation method of hafnium boride powder.
Background
Hafnium boride (HfB)2) The material has a series of unique excellent performances such as high melting point (3250 ℃), high hardness (39GPa), high conductivity (15 omega. cm), low oxidation rate and high chemical stability, and can be widely applied to industries such as engines, advanced aircrafts, plasma discharge bodies, cutting tools, hearth elements and the like as a key raw material of a high-temperature structural material (a thermal protection structural material which can still maintain chemical and physical stability under an ultrahigh-temperature aerobic environment with the temperature of more than 2000 ℃), so that the material attracts much attention in recent years. Purity and particle size are key factors affecting hafnium boride applications.
In the prior art, raw materials are processed by grinding in the course of preparing finished products, so as to form powdery materials, and are sieved according to the powdery materials. However, the powdery material is easy to lose in the processing process, and the screening process is poor, so that the purity of the prepared hafnium boride cannot reach the standard.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of hafnium boride powder, so as to improve the purity of the prepared hafnium boride powder.
In order to achieve the purpose, the invention provides the following scheme:
a preparation method of hafnium boride powder comprises the following steps:
mixing the raw materials, primarily grinding, primarily drying and pressing into blocks; the raw materials comprise hafnium oxide, boron carbide and carbon black;
carrying out vacuum synthesis on the block to obtain a semi-finished product;
crushing, primary sieving, secondary drying and secondary sieving are carried out on the semi-finished product to obtain finished product powder; the time of the secondary drying is determined by the particle size of the semi-finished product.
Preferably, after the vacuum synthesis of the block to obtain a semi-finished product, the method further includes:
sampling the semi-finished product to obtain a sample;
carrying out infrared and element analysis on the sample to obtain analysis index information;
and judging according to the analysis index information and qualified index information, and if the analysis index information does not accord with the qualified index information, terminating the preparation process of the hafnium boride powder.
Preferably, after the semi-finished product is crushed, primarily sieved, secondarily dried, and secondarily sieved to obtain a finished product powder, the method further includes:
performing quality detection on the finished product powder to obtain qualified powder and unqualified powder;
and warehousing and storing the qualified powder.
Preferably, the ratio of the hafnium oxide, the boron carbide and the carbon black is 20: 3: 1.6.
preferably, the purity of the hafnium oxide is more than 99%, the average particle size of the hafnium oxide is 2-3 μm, and the content of metal elements in the hafnium oxide is less than 0.1%;
the purity of the boron carbide is more than 99%, the average particle size range of the boron carbide is 2-3 mu m, and the content of metal elements in the boron carbide is less than 0.1%;
the purity of the carbon black is more than 99%, and the average particle size range of the carbon black is 2-3 mu m.
Preferably, the mixing is performed for a time ranging from 235 minutes to 245 minutes.
Preferably, the temperature range of the primary drying is 60-80 degrees, and the operation time of the primary drying is 120 minutes.
Preferably, the heating temperature range of the vacuum synthesis is 2400-2600 degrees, the temperature rise time range of the vacuum synthesis is 3-4 hours, the reaction time of the vacuum synthesis is 4 hours, and the reaction vessel of the vacuum synthesis is an isostatic pressure graphite crucible.
Preferably, the primary screening is a water screen, and the water screen is used for carrying out secondary grading on the semi-finished product; the secondary screening is manual screening.
Preferably, the operation time of the secondary drying is 600 minutes.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention provides a preparation method of hafnium boride powder, which can obtain the hafnium boride powder with high purity and ultra-fine granularity according to the operation flows of sequentially mixing, primary grinding, primary drying, vacuum synthesis, crushing, primary sieving, secondary drying and secondary sieving of raw materials, and discloses a secondary drying process and a secondary sieving process, wherein the product is dried into blocks after being mixed and ground in the primary drying process, so that the raw material loss caused by vacuumizing is prevented, and the ball milling time of the synthesized powder preparation in the secondary sieving process is adjusted according to the required granularity condition, so that products with different granularities are produced, and the degree of the granularity is also ensured. That is, the present invention can improve not only the purity of the prepared hafnium boride powder but also the fineness of the particle size of the prepared hafnium boride powder.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a flow chart of a preparation method in an embodiment provided by the present invention;
fig. 2 is a schematic process flow diagram in an embodiment provided by the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
The terms "first," "second," "third," and "fourth," etc. in the description and claims of this application and in the accompanying drawings are used for distinguishing between different objects and not for describing a particular order. Furthermore, the terms "include" and "have," as well as any variations thereof, are intended to cover non-exclusive inclusions. For example, the inclusion of a list of steps, processes, methods, etc. is not limited to only those steps recited, but may alternatively include additional steps not recited, or may alternatively include additional steps inherent to such processes, methods, articles, or devices.
The invention aims to provide a preparation method of hafnium boride powder, which can improve the purity of the prepared hafnium boride powder.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Fig. 1 is a flow chart of a preparation method in an embodiment provided by the present invention, and as shown in fig. 1, the present invention provides a preparation method of hafnium boride powder, including:
a preparation method of hafnium boride powder comprises the following steps:
step 100: mixing the raw materials, primarily grinding, primarily drying and pressing into blocks; the raw materials comprise hafnium oxide, boron carbide and carbon black;
step 200: carrying out vacuum synthesis on the block to obtain a semi-finished product;
step 300: crushing, primary sieving, secondary drying and secondary sieving are carried out on the semi-finished product to obtain finished product powder; the time of the secondary drying is determined by the particle size of the semi-finished product.
Fig. 2 is a schematic process flow diagram in an embodiment provided by the present invention, and as shown in fig. 2, before the step of "mixing raw materials" (mixing raw materials in the figure) is performed in this embodiment, the present invention further includes production preparation work, where the production preparation work includes detecting equipment indexes, electricity and water are normal.
Preferably, after the step 200, the method further includes:
sampling the semi-finished product to obtain a sample;
carrying out infrared and element analysis on the sample to obtain analysis index information;
and judging according to the analysis index information and qualified index information, and if the analysis index information does not accord with the qualified index information, terminating the preparation process of the hafnium boride powder.
Specifically, the sample is subjected to X-ray diffraction (xrd) analysis, the structure and the component proportion of the product are confirmed to be correct, if the structure and the component proportion are correct, the preparation is continued, and if the structure and the component proportion are incorrect, the preparation process is stopped.
Preferably, after the semi-finished product is crushed, primarily sieved, secondarily dried, and secondarily sieved to obtain a finished product powder, the method further includes:
performing quality detection on the finished product powder to obtain qualified powder and unqualified powder;
and warehousing and storing the qualified powder.
Specifically, before starting the operation, the technician needs to carefully learn the process files according to the requirements of the process files and confirm each step in the process. And a technician and a field operator check the linking condition of the instrument and equipment together to ensure that the instrument and equipment operate normally. The technical personnel take the raw materials required by production and register the corresponding specification quantity in the warehouse entry list and the production record list. The contents of the instrument and equipment according to the present embodiment are as shown in table 1.
TABLE 1
| Serial number | Name (R) | Model number | Number of | Use of | Remarks for note |
| 1 | Vacuum sintering furnace | HS-FVHS4/4/10 | 1 | High temperature treatment | 2600° |
| 2 | Ball mill | Non-standard homemade | 1 | Grinding treatment | |
| 3 | Particle size classifier | Non-standard homemade | 1 | Screening process | Micron-millimeter |
| 4 | Spiral mixer | WLDH-0.5 | 1 | Mixing of raw materials | |
| 5 | Drying cabinet | Non-standard homemade | 1 | Drying treatment | |
| 6 | Detecting instrument | LT2100 | 1 | Detecting particle size | 100nm-2000um |
Optionally, the vacuum sintering furnace is applied to a vacuum synthesis process, the ball mill is applied to a secondary screening process, the particle size classifier is applied to a primary screening process, the spiral mixer is applied to a mixing process, the drying box is applied to a primary drying process and a secondary drying process, and the detector is applied to an infrared and element analysis process and a quality detection process.
Preferably, the ratio of the hafnium oxide, the boron carbide and the carbon black is 20: 3: 1.6.
preferably, the purity of the hafnium oxide is more than 99%, the average particle size of the hafnium oxide is 2-3 μm, and the content of metal elements in the hafnium oxide is less than 0.1%;
the purity of the boron carbide is more than 99%, the average particle size range of the boron carbide is 2-3 mu m, and the content of metal elements in the boron carbide is less than 0.1%;
the purity of the carbon black is more than 99%, and the average particle size range of the carbon black is 2-3 mu m.
The raw material information table in this example is shown in table 2.
TABLE 2
| Serial number | Name (R) | Specification of | Unit of measurement | Dosage of | Remarks for note |
| 1 | Carbon black powder | Powder of | Kilogram (kilogram) | ||
| 2 | Hafnium oxide | Powder of | Kilogram (kilogram) | An inlet | |
| 3 | Boron carbide | Powder of | Kilogram (kilogram) |
Optionally, in the vacuum synthesis process of this embodiment, it should be noted that the running state of the apparatus is observed at regular time during the temperature raising process, and a record is made, and an isostatic pressure graphite crucible is used.
The specification requirements of the raw materials in this example are shown in table 3.
TABLE 3
Preferably, the mixing is performed for a time ranging from 235 minutes to 245 minutes.
Preferably, the temperature range of the primary drying is 60-80 degrees, and the operation time of the primary drying is 120 minutes.
Preferably, the heating temperature range of the vacuum synthesis is 2400-2600 degrees, the temperature rise time range of the vacuum synthesis is 3-4 hours, the reaction time of the vacuum synthesis is 4 hours, and the reaction vessel of the vacuum synthesis is an isostatic pressure graphite crucible.
Preferably, the primary screening is a water screen, and the water screen is used for carrying out secondary grading on the semi-finished product; the secondary screening is manual screening.
Specifically, during secondary screening, the milling time can be adjusted according to the required granularity condition for the powder process after synthesis, and manual screening is carried out through the selection of a crushing filter screen, the secondary screening needs specific personnel to operate, the milling process utilizes a ball mill to carry out the grinding of granularity, and the longer the grinding time, the smaller the granularity.
Specifically, if powder of 1 to 3um is required, grinding is carried out for 2 hours. If 3-5um powder is required, 1 hour of milling is required.
The specifications of the auxiliary materials in this example are shown in table 4.
TABLE 4
| Serial number | Name (R) | Technical index | Remarks for note |
| 1 | Crucible pot | Isostatic pressing phi 30cm 35cm | High-purity graphite |
| 3 | Gloves | The material is as follows: acetonitrile without powder | Ames is an example of |
| 4 | Gauze mask | Dust prevention | 3M |
| 5 | Stainless steel sieve | 304 steel |
Specifically, the gloves and the mask are worn on the body surfaces of technicians and operators, and the stainless steel screen is used in a primary screening process or a secondary screening process.
Preferably, the operation time of the secondary drying is 600 minutes.
The process flow of this example is shown in Table 5.
The invention has the following beneficial effects:
(1) the invention introduces primary drying and secondary drying, thereby avoiding the defect that the purity of the final product is reduced due to the introduction of water in the prior art, and further improving the purity of the product.
(2) The dried blocky product can avoid the deviation of the component proportion of the product caused by the loss of raw materials due to vacuumizing in the subsequent production process, thereby improving the accuracy of the proportion of the prepared finished product.
(3) The invention adjusts the ball milling time according to the required granularity condition of the synthesized powder preparation in the secondary sieving process, thereby producing products with different granularities and ensuring the fineness degree of the granularity.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A preparation method of hafnium boride powder is characterized by comprising the following steps:
mixing the raw materials, primarily grinding, primarily drying and pressing into blocks; the raw materials comprise hafnium oxide, boron carbide and carbon black;
carrying out vacuum synthesis on the block to obtain a semi-finished product;
crushing, primary sieving, secondary drying and secondary sieving are carried out on the semi-finished product to obtain finished product powder; the time of the secondary drying is determined by the particle size of the semi-finished product.
2. The method according to claim 1, wherein the vacuum synthesis of the block to obtain a semi-finished product further comprises:
sampling the semi-finished product to obtain a sample;
carrying out infrared and element analysis on the sample to obtain analysis index information;
and judging according to the analysis index information and qualified index information, and if the analysis index information does not accord with the qualified index information, terminating the preparation process of the hafnium boride powder.
3. The preparation method according to claim 1, wherein the crushing, primary sieving, secondary drying and secondary sieving of the semi-finished product to obtain a finished powder further comprises:
performing quality detection on the finished product powder to obtain qualified powder and unqualified powder;
and warehousing and storing the qualified powder.
4. The preparation method according to claim 1, wherein the ratio of the hafnium oxide, the boron carbide and the carbon black is 20: 3: 1.6.
5. the preparation method according to claim 1, wherein the purity of the hafnium oxide is > 99%, the average particle size of the hafnium oxide is in the range of 2-3 μm, and the content of metal elements in the hafnium oxide is < 0.1%;
the purity of the boron carbide is more than 99%, the average particle size range of the boron carbide is 2-3 mu m, and the content of metal elements in the boron carbide is less than 0.1%;
the purity of the carbon black is more than 99%, and the average particle size range of the carbon black is 2-3 mu m.
6. The method of claim 1, wherein the mixing is performed for a time period ranging from 235 minutes to 245 minutes.
7. The method according to claim 1, wherein the temperature range of the primary drying is 60 ° to 80 °, and the operation time of the primary drying is 120 minutes.
8. The preparation method according to claim 1, wherein the heating temperature of the vacuum synthesis ranges from 2400 ° to 2600 °, the temperature rise time of the vacuum synthesis ranges from 3 to 4 hours, the reaction time of the vacuum synthesis ranges from 4 hours, and the reaction vessel of the vacuum synthesis is an isostatic graphite crucible.
9. The method for preparing the semi-finished product according to claim 1, wherein the primary screening is a water screen for secondary classification of the semi-finished product; the secondary screening is manual screening.
10. The method according to claim 1, wherein the secondary drying is performed for 600 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111200190.8A CN113816392A (en) | 2021-10-14 | 2021-10-14 | Preparation method of hafnium boride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111200190.8A CN113816392A (en) | 2021-10-14 | 2021-10-14 | Preparation method of hafnium boride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113816392A true CN113816392A (en) | 2021-12-21 |
Family
ID=78916766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111200190.8A Pending CN113816392A (en) | 2021-10-14 | 2021-10-14 | Preparation method of hafnium boride powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113816392A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AUPM933094A0 (en) * | 1994-11-08 | 1994-12-01 | Australian National University, The | Production of borides |
| CN101428812A (en) * | 2008-09-19 | 2009-05-13 | 中国科学院上海硅酸盐研究所 | Synthesis of high-purity hafnium boride powder |
| CN103754891A (en) * | 2014-01-09 | 2014-04-30 | 航天材料及工艺研究所 | Method for preparing hafnium boride powder by using boron/carbothermic method |
| CN106276941A (en) * | 2016-08-26 | 2017-01-04 | 洛阳金鹭硬质合金工具有限公司 | A kind of preparation method of molybdenum boride powder |
| CN107200585A (en) * | 2017-05-04 | 2017-09-26 | 武汉科技大学 | Long bar-shaped hafnium boride powder of one kind and preparation method thereof |
| CN107986290A (en) * | 2017-12-30 | 2018-05-04 | 湖南人文科技学院 | A kind of preparation method of chromium boride powder |
| WO2020077771A1 (en) * | 2018-10-15 | 2020-04-23 | 广东工业大学 | Ultrafine high-entropy solid-melt powder, preparation method therefor and application thereof |
| CN112919913A (en) * | 2021-03-16 | 2021-06-08 | 矿冶科技集团有限公司 | Preparation method of high-purity superfine hafnium boride powder and hafnium boride powder |
| US20210179499A1 (en) * | 2018-12-23 | 2021-06-17 | Shanghai Jiao Tong University | METHOD FOR PREPARATION OF DENSE HfC(Si)-HfB2 COMPOSITE CERAMIC |
-
2021
- 2021-10-14 CN CN202111200190.8A patent/CN113816392A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AUPM933094A0 (en) * | 1994-11-08 | 1994-12-01 | Australian National University, The | Production of borides |
| CN101428812A (en) * | 2008-09-19 | 2009-05-13 | 中国科学院上海硅酸盐研究所 | Synthesis of high-purity hafnium boride powder |
| CN103754891A (en) * | 2014-01-09 | 2014-04-30 | 航天材料及工艺研究所 | Method for preparing hafnium boride powder by using boron/carbothermic method |
| CN106276941A (en) * | 2016-08-26 | 2017-01-04 | 洛阳金鹭硬质合金工具有限公司 | A kind of preparation method of molybdenum boride powder |
| CN107200585A (en) * | 2017-05-04 | 2017-09-26 | 武汉科技大学 | Long bar-shaped hafnium boride powder of one kind and preparation method thereof |
| CN107986290A (en) * | 2017-12-30 | 2018-05-04 | 湖南人文科技学院 | A kind of preparation method of chromium boride powder |
| WO2020077771A1 (en) * | 2018-10-15 | 2020-04-23 | 广东工业大学 | Ultrafine high-entropy solid-melt powder, preparation method therefor and application thereof |
| US20210179499A1 (en) * | 2018-12-23 | 2021-06-17 | Shanghai Jiao Tong University | METHOD FOR PREPARATION OF DENSE HfC(Si)-HfB2 COMPOSITE CERAMIC |
| CN112919913A (en) * | 2021-03-16 | 2021-06-08 | 矿冶科技集团有限公司 | Preparation method of high-purity superfine hafnium boride powder and hafnium boride powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xu et al. | Fourier transform infrared spectroscopy data and carbon isotope characteristics of the ophiolite-hosted diamonds from the Luobusa ophiolite, Tibet, and Ray-Iz ophiolite, Polar Urals | |
| Radousky et al. | Preparation and Raman analysis of single-phase Y 1− x Pr x Ba 2 Cu 3 O 7− δ | |
| CN102041402A (en) | Preparation method of low-oxygen molybdenum alloy and application thereof | |
| CN102583346B (en) | Method for preparing special graphite | |
| CN107867690B (en) | A kind of high temperature base WC powder and its preparation method and application | |
| CN109794598B (en) | Preparation method of ultra-pure rhenium ingot | |
| CN1275532A (en) | Productive method for converting uranium metal alloy into UO2 powder and core block | |
| CN102041403A (en) | Preparation method of low-oxygen MHC alloy and application of low-oxygen MHC alloy | |
| CN113816392A (en) | Preparation method of hafnium boride powder | |
| CN107973299B (en) | Production system and production process of high-temperature-base WC powder | |
| CN106756091A (en) | A kind of extracting method of Metals of Discarded Printed Circuit Boards copper | |
| CN108946775A (en) | Alpha-alumina powder, preparation method and application | |
| CN113697816A (en) | Preparation method of silicon powder | |
| CN110668820A (en) | Preparation method of high-performance carbon graphite product with superfine structure | |
| CN105645473A (en) | Preparation system and method for blue tungsten with fine particles | |
| CN112504778B (en) | Energy-containing tungsten alloy standard substance and preparation method thereof | |
| CN104724749B (en) | A kind of method for producing ultrafine copper oxide powder | |
| CA1115066A (en) | Process for the production of extra fine cobalt powder | |
| CN104261398B (en) | Raw material for preparing graphene and preparation method thereof | |
| CN114813427A (en) | Method for testing wear resistance of carbon material | |
| CN102175557B (en) | Method for testing trace impurities in ultrahigh-purity graphite | |
| CN110180662A (en) | The preparation process of schmigel | |
| Ferreira et al. | A model for the behavior of thorium uranium mixed oxide kernels in the pelletizing process | |
| CN108892140A (en) | A kind of method that vacuum method prepares carbon titanium carbonitride powder | |
| CN110697774B (en) | Method for preventing tantalum-niobium material from caking in sintering process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |