JPS6212604A - Synthesis of ditungsten monocarbide - Google Patents
Synthesis of ditungsten monocarbideInfo
- Publication number
- JPS6212604A JPS6212604A JP60150166A JP15016685A JPS6212604A JP S6212604 A JPS6212604 A JP S6212604A JP 60150166 A JP60150166 A JP 60150166A JP 15016685 A JP15016685 A JP 15016685A JP S6212604 A JPS6212604 A JP S6212604A
- Authority
- JP
- Japan
- Prior art keywords
- ditungsten
- monocarbide
- raw material
- tungsten oxide
- alkali metal
- 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
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔発明の利用分用〕
本発明は、−炭化二タングステン（ＷＺＣ）の合成法に
係り、特にその粉体を得るのに好適な方法である。DETAILED DESCRIPTION OF THE INVENTION [Uses of the Invention] The present invention relates to a method for synthesizing tungsten carbide (WZC), and is particularly a method suitable for obtaining powder thereof.
従来のＷ２０合成法は、タングステン金属粉とカーボン
ブラックを２：１に混合したものを１４００〜１７００
℃で固相反応させるもので、高温を必要とした。低温で
合成するには酸化タングステン粉を約７００℃でＣＯに
よって炭化する方法が考えられるが、この方法では、Ｗ
Ｃが主として生成され、反応を中間のＷ２Ｃで止めるこ
とは困難であった。The conventional W20 synthesis method uses a mixture of tungsten metal powder and carbon black at a ratio of 1,400 to 1,700
The solid phase reaction was carried out at ℃ and required high temperatures. One possible method for synthesis at low temperatures is to carbonize tungsten oxide powder at about 700°C with CO;
C was mainly produced, and it was difficult to stop the reaction at intermediate W2C.
なお関連する文献に英国特許１３４７５３４がある。A related document is British Patent No. 1347534.
本発明の目的は、９００℃以下のような低温で粒径約１
μｍのＷ２Ｃ粉を提供することにある。The object of the present invention is to obtain particles with a particle size of about 1 at low temperatures, such as below 900°C.
Our objective is to provide μm W2C powder.
粒径１μｍ以下のタングステンカーバイド（ｗＣ）粉の
合成法は公知もある（英国特許翫１３４７５３４．１９
７０．６．４）、これはタングステン酸化物を７００℃
以下でＣＯで炭化する方法であるが、この方法ではＷ、
Ｃはきわめてわずかしか生成しない。本発明は原料のタ
ングステン酸化物にアルカリ金属塩を加えることによっ
て生成物の主成分をＷ、Ｃとするものである。There is a known method for synthesizing tungsten carbide (wC) powder with a particle size of 1 μm or less (UK Patent No. 1347534.19).
70.6.4), which means that tungsten oxide is heated to 700°C.
The following is a method of carbonizing with CO, but in this method W,
C produces very little. In the present invention, the main components of the product are W and C by adding an alkali metal salt to tungsten oxide as a raw material.
以下、本発明の実施例を述べる。 Examples of the present invention will be described below.
実施例１
タングステン酸４６．４ ｇを１５％のアンモニア水溶
液２５０ｍΩに、５０〜７０℃の温度において完全に溶
解させた。不溶の不純物をろ過にて除いた液を蒸発乾固
したものをカリウム（Ｋ）なしの原料粉ということにす
る。一方、上記と同様の液に１．２ｇ の水酸化カリウ
ムを溶かした液を蒸発乾固したものをカリウム（Ｋ）あ
りの原料粉ということにする。なお、ＫとＷとの原子比
は０．１ である。Example 1 46.4 g of tungstic acid was completely dissolved in 250 mΩ of a 15% aqueous ammonia solution at a temperature of 50 to 70°C. The liquid from which insoluble impurities have been removed by filtration is evaporated to dryness and is referred to as potassium (K)-free raw material powder. On the other hand, a solution obtained by dissolving 1.2 g of potassium hydroxide in the same solution as above and evaporating it to dryness is referred to as a raw material powder containing potassium (K). Note that the atomic ratio between K and W is 0.1.
上記２種の原料粉をそれぞれ１ｇとって、８００℃毎分
１００ｍＱのＣＯの条件で０．５，１．２時間と反応時
間を変えて反応させた結果、表１が得られた。Ｋなし原
料粉を用いて０．５ 時間で炭化させたものは、結晶性
が悪く、種々のＷ酸化物を金弟１表、生成物の組成、（
）内の数値は生成比率んでいた。表から、次のようなこ
とがわかる。１ｇの原料粉を８００℃で炭化させたとき
、Ｋなしの原料粉からはＷ２Ｃが収率よく得られないの
に対し、Ｋありの原料粉からは、Ｗ２Ｃのような中間生
成物が収率よく得られる。また、炭化時間にも最適値が
存在し、１．０時間のときにＷ２Ｃの生成比率が８０％
にも達する。表面積から、粒径を推測すると約１．０
μｍであった。Table 1 was obtained as a result of taking 1 g of each of the above two types of raw material powders and reacting them at 800° C. with CO at 100 mQ/min for 0.5 and 1.2 hours. The product carbonized for 0.5 hours using K-free raw material powder had poor crystallinity, and various W oxides were
) is the production ratio. From the table, we can see the following: When 1 g of raw material powder is carbonized at 800°C, W2C cannot be obtained in good yield from raw material powder without K, whereas intermediate products such as W2C are obtained from raw material powder with K in good yield. well obtained. In addition, there is an optimum value for carbonization time, and at 1.0 hours, the W2C generation ratio is 80%.
reach even. Estimating the particle size from the surface area is approximately 1.0
It was μm.
実施例２
実施例１にて記したＫありの原料粉を用いて７００℃か
ら１０００℃の炭化温度で合成した。その結果、７００
℃では２時間反応させてもＷＯ□が主成分であり、さら
に長時間反応させるとＷＣ成分が増加した。１０００℃
ではＷＣが主成分となった。Example 2 Synthesis was carried out using the K-containing raw material powder described in Example 1 at a carbonization temperature of 700°C to 1000°C. As a result, 700
At C., WO□ was the main component even after 2 hours of reaction, and when the reaction was continued for a longer time, the WC component increased. 1000℃
In this case, WC was the main component.
９００℃では反応時間を短かくすることによってＷ２Ｃ
の生成比率を６０％とすることができた。At 900℃, by shortening the reaction time, W2C
The production ratio of 60% was achieved.
したがって炭化反応温度は７５０〜９００℃にするのが
適当である。Therefore, it is appropriate that the carbonization reaction temperature be 750 to 900°C.
実施例３
に含有率（Ｗに対するＫの原子比率）の異なる原料粉を
実施例１と同様に調製した。Ｋ含有率は０．００５．０
．０１．０．１．１．０．１０．２０ トした。Example 3 Raw material powders having different contents (atomic ratio of K to W) were prepared in the same manner as in Example 1. K content is 0.005.0
．． 01.0.1.1.0.10.20
その結果、Ｋ含有率０．０１，０．１，１．０．ＩＱ（
７）原料粉から炭化した場合にのみ、Ｗ２Ｃ生成に有利
に働いていることが見出された。As a result, the K content was 0.01, 0.1, 1.0. IQ(
7) It was found that only when carbonization is performed from raw material powder, it works favorably for W2C production.
実施例４
実施例１においてＫありの原料粉を作る際に、水酸化カ
リウムのかわりに、炭酸カリウム（Ｋｚ ｃ Ｏ３）
、塩化カリウム（ＫＣＱ）、または塩化ナトリウム（Ｎ
ａＣｆｌ）を用いても実施例１と同様の効果があった。Example 4 When making the raw material powder containing K in Example 1, potassium carbonate (Kz c O3) was used instead of potassium hydroxide.
, potassium chloride (KCQ), or sodium chloride (N
aCfl) had the same effect as in Example 1.
またＫなしの原料粉に炭酸カリウムを機械的に混合した
ものでも同様の効果があった。したがってタングステン
酸化物にアルカリ金属化合物を含ませることによって１
ｗ２Ｃを生成比率よく合成できることになる。A similar effect was also obtained when potassium carbonate was mechanically mixed with the raw material powder without K. Therefore, by including an alkali metal compound in tungsten oxide, 1
This means that w2C can be synthesized with a good production ratio.
本発明によれば、７５０〜９００℃という比較的低温で
Ｗ２Ｃ粉が収率よく合成できる効果がある。According to the present invention, W2C powder can be synthesized in good yield at a relatively low temperature of 750 to 900°C.
Claims (1)
ンに対する原子比０．０１から１０の割合で混合したの
ち、温度７５０〜９００℃で一酸化炭素と反応させるこ
とを特徴とする一炭化二タングステンの合成法。A method for synthesizing ditungsten monocarbide, which comprises mixing tungsten oxide with an alkali metal compound at an atomic ratio of 0.01 to 10 to tungsten, and then reacting the mixture with carbon monoxide at a temperature of 750 to 900°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60150166A JPS6212604A (en) | 1985-07-10 | 1985-07-10 | Synthesis of ditungsten monocarbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60150166A JPS6212604A (en) | 1985-07-10 | 1985-07-10 | Synthesis of ditungsten monocarbide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6212604A true JPS6212604A (en) | 1987-01-21 |
Family
ID=15490947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60150166A Pending JPS6212604A (en) | 1985-07-10 | 1985-07-10 | Synthesis of ditungsten monocarbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6212604A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4976294A (en) * | 1988-06-13 | 1990-12-11 | Yazaki Corporation | Method and apparatus for making specified-length wires for wire harness |
-
1985
- 1985-07-10 JP JP60150166A patent/JPS6212604A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4976294A (en) * | 1988-06-13 | 1990-12-11 | Yazaki Corporation | Method and apparatus for making specified-length wires for wire harness |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4794620B2 (en) | Circulation method for producing lithium metal phosphate by wet chemical method | |
| KR19990021989A (en) | Spherical aggregated basic cobalt carbonate (II) and spherical aggregated cobalt hydroxide (II), preparation method thereof and use thereof | |
| CN1796029B (en) | Fine tungsten carbide powder | |
| JP3202987B2 (en) | Manufacturing method of titanium carbide whisker | |
| Stoyanova et al. | Synthesis and structural characterization of MoO3 phases obtained from molybdic acid by addition of HNO3 and H2O2 | |
| CN110997562A (en) | Process for the preparation of vanadium phosphate | |
| JPS6212604A (en) | Synthesis of ditungsten monocarbide | |
| JPH11189410A (en) | Production of hauyne | |
| JP2502572B2 (en) | Solid lactate salt and method for producing the same | |
| DE3781549T2 (en) | METHOD FOR PRODUCING CERAMIC POWDER. | |
| JP3867234B2 (en) | Slightly soluble condensed melamine phosphate and method for producing the same | |
| US1389862A (en) | Manufacture of potassium sulfate | |
| Steigerwalt et al. | Preparation of graphitic carbon nanofibers with the use of water-soluble supports | |
| JP2834199B2 (en) | Method for producing ultrafine tungsten particles | |
| RU2455377C2 (en) | Method to produce metal-boride composite powders of molybdene and tungsten | |
| JPS58213617A (en) | Production of titanium carbonitride powder | |
| KR20050013990A (en) | Process for manufactruing diamond using a novel method of catalysis and a new method for processing the graphite and catalyst mixture used in synthesis | |
| JP4023711B2 (en) | Method for producing high purity fine tungsten carbide powder without the need for a grinding step | |
| JPS61132509A (en) | Production of silicon carbide | |
| JPH049732B2 (en) | ||
| JPH02271919A (en) | Production of fine powder of titanium carbide | |
| US524470A (en) | Half to charles y | |
| US1281118A (en) | Process for manufacturing oxalates. | |
| Amosov et al. | Self-propagating high-temperature synthesis of titanium carbide nanopowder from the granulated charge | |
| JPS58115016A (en) | Preparation of fine powdery silicon carbide |