CN1015238B - Preparation method for tungsten cerium powder - Google Patents
Preparation method for tungsten cerium powderInfo
- Publication number
- CN1015238B CN1015238B CN 89107270 CN89107270A CN1015238B CN 1015238 B CN1015238 B CN 1015238B CN 89107270 CN89107270 CN 89107270 CN 89107270 A CN89107270 A CN 89107270A CN 1015238 B CN1015238 B CN 1015238B
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- tungsten
- cerium
- powder
- reduction
- preparation
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention relates to a method for preparing tungsten cerium powder, which comprises: a cerium acetate solution is added in tungsten trioxide or ammonium paratungstate (WO3 is obtained after calcination at the temperature of 800 to 850 DEG C) to be stirred, then the tungsten trioxide or the ammonium paratungstate is evaporated and concentrated at high pressure and dried, and after second reduction and screening, the tungsten cerium powder with 1 to 8 wt% of cerium dioxide in the tungsten base is obtained. The method for preparing tungsten cerium powder of the present invention solves the problem of environmental pollution in the process of past tungsten cerium powder preparation, the initial tungsten cerium powder containing 1 to 8 wt% of cerium dioxide prepared by the method of the present invention can be prepared into tungsten cerium electrode materials containing 1.0 to 6.0 wt% of cerium dioxide so that the difficult processing of tungsten cerium electrode materials containing more than 1.0% of cerium dioxide is overcome, and a substantive material breakthrough is made in the range of tungsten cerium electrode materials of 4 to 6%.
Description
The present invention relates to preparation method for tungsten cerium powder, belong to field of powder metallurgy.
As everyone knows, the electrode materials of the prepared one-tenth of applied powder metallurgy method, electrodes such as thorium tungsten, zirconium tungsten, tungsten cerium are arranged, it is mainly used in argon arc welding, fields such as plasma cutting, yet general traditional preparation process method, be to adopt in the WO3 powder, to add thorium nitrate 99.99004323A8urity solution, though, they all have lower electron work functon and high emitting performance, but adding Thorotrast in tungsten powder is to have serious radioactivity, can cause the harm of serious cumulated activity to human body, and certain difficulty is arranged in scale production.Second kind of preparation method is the disclosed a kind of method of Chinese patent application CN85100484A, this method is to add cerous nitrate solution to prepare tungsten cerium powder in tungstic oxide, though this method can be avoided radioactive harm, but be difficult to eliminate the pollution of nitrogen peroxide to environment, the third preparation method adds three ceria oxide powders to carry out mechanically mixing in tungsten powder, this method no doubt can be eliminated above-mentioned pollution problem, but owing to limited by the blended method, so the degree of scatter of cerium oxide particles in the tungsten base is not good enough, therefore caused very big difficulty to processing, thereby also use properties has been caused bad influence, electrode is prone to the drift of arc in welding process, makes the inaccessible relevant technologies standard-required of quality of weldment.
At the shortcoming that exists in the above-mentioned prior art, the inventor has proposed a kind of preparation method of tungsten cerium powder of novelty, use this method and not only solved tungsten-cerium electrode pollution problem in manufacturing processed, but also solved the difficult point of electrode in each leading indicators such as processing and use propertieies, manufacturing provides one, the approach of simple and direct low consumption to tungsten-cerium electrode again simultaneously.Adopt the tungsten cerium powder of the present invention's preparation, just can prepare the tungsten-cerium electrode of the different trades mark with ordinary method.
The preparation method of tungsten cerium powder of the present invention is: add cerous acetate solution in tungstic oxide or ammonium paratungstate (promptly becoming WO3 after 800-850 ℃ of roasting), stirred then 5-10 minute, high-pressure evaporation concentrates, evaporating pressure is the 2.2-2.4 normal atmosphere, oven dry, bake out temperature is 240-260 ℃, at last in logical hydrogen tubulose reduction furnace through once, secondary reduction, reduction temperature is 650-670 ℃ for the first time, reduction temperature is 960-980 ℃ for the second time, and the tungsten cerium powder after the reduction just can be prepared the fine tungsten cerium powder that is evenly distributed of cerium oxide particle by 120 mesh sieves.Can prepare cerium oxide content with the inventive method is that 1-8%(is heavy) tungsten-cerium powder, using this tungsten-cerium powder former powder, can to prepare cerium oxide content be that 1-6%(is heavy) W-Ce electrode material.
Fig. 1 is tungsten cerium square billet (WCe20) the transverse section metallograph of cerous acetate method preparation of the present invention.
Fig. 2 is tungsten cerium square billet (WCe20) the transverse section metallograph that mechanical mixing is produced.
The following examples are that the present invention is further described, rather than limitation of the present invention.
The preparation of preparation of embodiment 1 2% tungsten cerium powder and tungsten-cerium electrode
(1) preparation of cerous acetate solution.
Get purity and be the cerous acetate crystal 4 .1kg more than 99.9%, join in 30 liters of deionized waters and at room temperature stirred 5-10 minute, treat that crystal all gets final product after the dissolving.
The doping of (2) 2% tungsten cerium powder
After 50 liters of deionized waters are joined evaporating pan, again the WO3 powder of 100kg is put into pot, carry out 5 minutes stirring, add the above-mentioned cerous acetate solution for preparing then, continue to stir, evaporation, evaporating pressure are 2.2-2.4 normal atmosphere, after to be evaporated the concentrating, dry with drying baker, bake out temperature be 250 ℃ during to complete drying till.
(3) reduction
In logical hydrogen reduction furnace, carry out the reduction of two-stage, reduction temperature is 660 ± 10 ℃ for the first time, recovery time is 30 a minutes/boat, reduction temperature is 970 ± 10 ℃ for the second time, recovery time is 40 a minutes/boat, used nickel boat charge amount is 250g during reduction, and contrary hydrogen direction is packed into, and the tungsten cerium powder after the reduction is crossed 120 sieves.
(4) compacting
The tungsten cerium powder that reduction is good carries out mixing in 4 hours, adds alcohol then, and the glycerine mixed solution carries out batch mixing, alcohol: glycerine=1: 7; Mixed solution: powder=2: 1, treat mixed after, suppress with 500 tons hydropress, pressing pressure is 3.5 tons/centimetre, pressed compact is of a size of 12 * 12 * 400(centimetre), carry out pre-burning then in molybdenum wire furnace, calcined temperature is 1200 ℃, be incubated after 30 minutes take out standby.
(5) incipient fusion
The base bar carries out high temperature sintering in the incipient fusion machine of logical hydrogen protection, the highest insulation electric current is 3050A, soaking time 30 minutes, and the ceria content of analysis metal base bar is generally about 2.0%.
(6) wire drawing of swaging
Tungsten-cerium electrode swaging from the square billet cogging to φ 3.1mm used the molybdenum wire furnace heating, and Heating temperature is respectively 1550 ℃; 1500 ℃.Carry out wire drawing then, wire drawing is temperature required to 2.4mm to be 1000 ℃.
The preparation of the tungsten-cerium raw powder of embodiment 2 8%
(1) cerous acetate solution produces the 1(1 with embodiment) identical.
(2) 15 liters deionized water and the cerous acetate solution for preparing are together joined in the evaporating pan, stir, after 3 minutes, the WO3 that adds 25kg stirs evaporation oven dry, other processing step and embodiment 1(2) identical.
(3) reduction, compacting, hammer melt, swage drawing step and embodiment 1(3) (4) (5) (6) are identical.
Tungsten cerium square billet cross section metallograph (Fig. 1) with the inventive method preparation is compared with the tungsten cerium square billet cross section metallograph (Fig. 2) of mechanical mixing preparation, can find out significantly, with the distribute distribution of cerium oxide in the electrode that is better than significantly the mechanical mixing preparation of the cerium oxide in the tungsten-cerium electrode of the inventive method preparation, and crystal is evenly tiny. Avoided simultaneously harmful gas that traditional nitric acid cerium addition method causes to the pollution of environment.
Claims (1)
1, a kind of preparation method of tungsten cerium powder, this method is included in adds cerous acetate solution in tungstic oxide or the ammonium paratungstate (being WO3 after 800-850 ℃ of roasting), stir then, high-pressure evaporation concentrates, oven dry, after once, secondary reduction also sieves, just can be equipped with the tungsten-cerium powder that in the tungsten base, contains 1-8% (weight) cerium oxide, it is characterized in that wherein said churning time is 5-10 minute, evaporating pressure is the 2.2-2.4 normal atmosphere, bake out temperature is 200-260 ℃, wherein once, secondary reduction carries out in logical hydrogen tubulose reduction furnace, reduction temperature is 650-670 ℃ for the first time, and reduction temperature is 960-980 ℃ for the second time, and filter with 120 mesh sieves the reduction back.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89107270 CN1015238B (en) | 1989-09-27 | 1989-09-27 | Preparation method for tungsten cerium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89107270 CN1015238B (en) | 1989-09-27 | 1989-09-27 | Preparation method for tungsten cerium powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1050511A CN1050511A (en) | 1991-04-10 |
| CN1015238B true CN1015238B (en) | 1992-01-01 |
Family
ID=4857129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89107270 Expired CN1015238B (en) | 1989-09-27 | 1989-09-27 | Preparation method for tungsten cerium powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1015238B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054563C (en) * | 1997-02-27 | 2000-07-19 | 北京钨钼材料厂 | Production method of lanthanum-tungsten electrode |
-
1989
- 1989-09-27 CN CN 89107270 patent/CN1015238B/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054563C (en) * | 1997-02-27 | 2000-07-19 | 北京钨钼材料厂 | Production method of lanthanum-tungsten electrode |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1050511A (en) | 1991-04-10 |
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Applicant after: Beijing Tungsten and Molybdenum Materials Factory Applicant before: Beijing High Smelting Metal Material Factory |
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Free format text: CORRECT: APPLICANT; FROM: BEIJING HIGH SMELTING METAL MATERIAL FACTORY TO: BEIJING TUNGSTEN + MOLYBDENUM MATERIAL FACTORY |
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