CN101462172A - Method for preparing diamond metal anchoring agent - Google Patents
Method for preparing diamond metal anchoring agent Download PDFInfo
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- CN101462172A CN101462172A CNA2009100640651A CN200910064065A CN101462172A CN 101462172 A CN101462172 A CN 101462172A CN A2009100640651 A CNA2009100640651 A CN A2009100640651A CN 200910064065 A CN200910064065 A CN 200910064065A CN 101462172 A CN101462172 A CN 101462172A
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Abstract
The invention provides a method for preparing a metallic bonding agent of diamond. In the method, oxalic acid is used as a precipitator; a parallel-flow coprecipitation method is applied to preparing a precursor; a simple reduction method of combining pyrolysis and hydrogen reduction is used to generate mixed metal powder; common hydrogen is passivated at normal temperature according to certain condition to obtain a high-purity evenly-mixed product which has a passivation layer with small oxygen content; the passivated product is placed for 5 to 15 days; and a temperature programmed reduction method is used to measure the oxygen content to be less than 0.4 percent. The method has simple operation; and the product has low oxygen content, good bonding force and can be used for preparing a diamond tool with excellent performance.
Description
Technical field
The invention belongs to and be used for the metallic bond technical field, be specifically related to a kind of preparation method of diamond metal anchoring agent alloyed powder.
Technical background
The effect of metal bond for diamond tools is fixed cutting element-diamond, and except that the plated metal bond, remaining all is to adopt powder metallurgic method to make.
Metallic bond has constituted the core of sintered diamond goods, and it is undertaking in the sintering instrument with bond matrix, control that diamond particles does not come off too early in the sintered body, consume and self constantly provide newborn diamond along effects such as grain swords.It bear huge impact hit with extrusion stress in, should have good cutting force and the maintenance instrument is complete, ideal situation is that the diamond of internal layer then constantly exposes out when the diamond on top layer wears away gradually, participate in cutting gradually, realize diamond tool normally from sharp.
At present, the method for preparing the diamond bond mainly contains two kinds: liquid phase method and solid phase method.Liquid phase preparation process mainly contains chemical coprecipitation, sol-gel process, spray pyrolysis, hydro-thermal method, microemulsion method, microwave-hydrothermal method, synthesis by shock wave, supercritical methanol technology and phase inversion etc.Solid phase method mainly contains: high energy mechanical is ground, self propagating high temperature is synthetic and low-temperature combustion synthesis etc.
Mechanical mixture and chemical coprecipitation are the common methods of preparation diamond bond, wherein chemical coprecipitation is meant in comprising the soluble-salt solution of two or more metal ion, add suitable precipitating reagent, metal ion is precipitated equably or crystallize out, again sediment dehydration-thermal decomposition-reduction is made metal alloy powders.Chemical coprecipitation from precipitation process also divide mix coprecipitation with and flow coprecipitation, the existing open report of correlation technique (diamond and grinding materials and grinding tool engineering, 2007 the 3rd phase P47～51).Can be divided into Several Methods such as hydroxide, oxalates, carbonate again by the precipitating reagent difference, be that 200510134575.3 invention " RE-containing prealloy powder " provides a kind of method that adopts oxalate method to prepare pre-alloyed powder as application number.
Because the metal powder that reduction obtains is oxidation easily in air, is necessary product is carried out surface passivation.Passivating method commonly used is: to by the metal powder that obtains after the general hydrogen reduction, switch feeding nitrogen and add an amount of oxygen or air in nitrogen, make reduzate form layer oxide film gradually on the surface.(application for a patent for invention prospectus, application number 200510107205.0) but this method add that the oxygen amount is wayward, and the passivation layer oxygen content of product is easily higher, and the step of switching has also increased the complexity of equipment and operation.
Summary of the invention
Purpose of the present invention is devoted to solve product and is prepared the problems referred to above that exist in the passivating process, proposing a kind of is precipitating reagent with oxalic acid, use and flow coprecipitation and prepare presoma, to add the easy method of reducing generation mixed metal powder that thermal decomposition combines with hydrogen reducing, carry out passivation by certain condition at normal temperatures with general hydrogen, the method for the diamond metal anchoring agent that obtain a kind of high-purity, mix, the passivation layer oxygen content is little.
Technical scheme of the present invention comprises the preparation mixing salt solution, and the stream coprecipitation makes and mix the oxalate precipitation thing, and is aging, washing, and the suction filtration dehydration, oven dry is decomposed, reduction, passivation such as packs at step.Be specially:
Get ferrous sulfate, nickelous sulfate and copper sulphate and at room temperature be mixed with mixing salt solution in the ratio of 5～6:3:1, the dissolving of principal goods material ferrous sulfate is controlled at 10～40% of saturation solubility;
Oxalic acid is made precipitating reagent, and its concentration is 1.0～1.5 times of salt-mixture total concentration, and with the pH value of NaOH conditioned reaction system, control method is oxalic acid and naoh concentration 1:1～3, and the volume of adding equates;
Place reactor to carry out equal-volume mixing salt solution and precipitating reagent and sodium hydroxide solution and flow co-precipitation, solution adding speed is 0.1～0.4Lmin
-1, reaction temperature is 20～100 ℃, and the reaction time is 0.3～2 hour, and the sediment ageing time is 12～24 hours, must mix the oxalate precipitation thing;
To mix the oxalate precipitation thing and filter, washing, 70～90 ℃ dry 6～10 hours down, heat up hydrogen gas space velocity 3000h at 200～600 ℃ of downstairs
-1, decomposition-reduction 5～11 hours;
With the article after the above-mentioned reduction, under general nitrogen atmosphere, carry out passivation, general hydrogen air speed is 1000h
-1～4000h
-1, passivation temperature is 10 ℃～200 ℃, passivation time is 2～12 hours, promptly gets product.
Product after the passivation was placed 5-15 days, measured its oxygen content with the temperature programmed reduction method and was lower than 4 ‰.
In the above-mentioned steps, precipitating reagent adopts oxalic acid, and does not use sodium oxalate, ammonium oxalate, has avoided sodium oxalate to bring more sodium ion into, increases the washing workload.And the oxalic acid cost is lower than ammonium oxalate; Adopt and stream coprecipitation preparation mixing oxalate precipitation, avoid certain composition part excessive, it is more even that each composition is mixed.
Because the oxalates heat decomposition temperature of three kinds of metallic irons, copper, nickel is all lower, and cupric oxalate and nickel oxalate major part directly be decomposed into elemental metals, and heating is then reduced when decomposing in hydrogen, the reduction rate quickening.And because the interaction between component makes the reduction of ferrous oxalate become easy.Mix oxalates most of reduction in the time of 480 ℃, in the time of 580 ℃, reduce fully.Under general nitrogen atmosphere, make reduzate cooling, at a lower temperature, the hydrogen reduction that do not recur, micro amount of oxygen wherein can be used for passivation on the contrary, adopts certain hydrogen gas space velocity and duration of ventilation can obtain the passivation product of less oxygen content.
The invention has the advantages that: do precipitating reagent with oxalic acid, use the presoma that stream coprecipitation also obtains the oxalates form, each component mixes, and is easily separated, easily decomposes, reduction, with passivation under certain condition under the general hydrogen normal temperature, easy and simple to handle and oxygen content is low.The alloy powder of this method preparation has good adhesion as diamond bond and diamond, can be used for the good diamond tool of processability.
The specific embodiment
The present invention is described in detail for following examples, but do not limit the present invention in any form.
Embodiment 1:
Get the principal goods material FeSO of Yuan material Chun Du ≧ 96%
47H
2The CuSO of O 28 Ke ， ≧ 98%
45H
2The NiSO of O15.3 Ke ， ≧ 98%
46H
2O 5.4 gram is mixed with volume and is 1 liter mixing salt solution, and the dissolving of principal goods material is controlled at 10% of saturation solubility;
Get the H of Yuan material Chun Du ≧ 99%
2C
2O
4H
2O is 1 liter a oxalic acid solution with per 23 gram dose volume, as precipitating reagent.Getting the NaOH of Yuan material Chun Du ≧ 99%, is 1 liter sodium hydroxide solution with per 7.2 gram dose volume, and mixing salt solution and precipitating reagent, sodium hydroxide solution are put into three head tanks;
And stream co-precipitation: under the normal temperature and pressure, open the head tank switch, with 0.2Lmin
-1Flow velocity, under the normal temperature and pressure by conduit with and the mode of stream mixing salt solution and precipitating reagent, NaOH introduced in the batch (-type) mechanical agitation reactor carried out coprecipitation reaction.50 ℃ of reaction temperatures, in 60 minutes reaction time, the sediment ageing time is 10 hours, must mix the oxalate precipitation thing;
With filter paper co-precipitation is filtered, filter cake is taken out spend deionised water then, filter with filter paper, washed twice gets final product;
Co-precipitation sample behind the filtration washing is placed baking oven, be controlled at 70～90 ℃, dry 6 hours;
Decomposition-reduction: the co-precipitation sample after will drying places the decomposition-reduction stove, and atmosphere is general hydrogen, and air speed is 3000h
-1, at first emptying 0.5h heats up afterwards, and in 200 ℃ of constant temperature 1.5h, 450 ℃ of constant temperature 2h, 600 ℃ of constant temperature 2h, programming rate are 10 ℃ of min
-1
After decomposition-reduction is finished, sample cooling under general hydrogen protection, general hydrogen air speed 1000h
-1Following passivation, passivation time are 12 hours, and 15 ℃ of temperature are treated to take out sample after passivation is finished from reaction tube.
The yield of metal component Fe, Cu, Ni is respectively 86.4%, 96.9%, 85.3%, places 15 days after the passivation, and measuring its oxygen content with the temperature programmed reduction method is 3.64 ‰.
Example 2:
Get the principal goods material FeSO of Yuan material Chun Du ≧ 96%
47H
2The CuSO of O 56 Ke ， ≧ 98%
45H
2The NiSO of O30.6 Ke ， ≧ 98%
46H
2O 10.8 gram is mixed with volume and is 1 liter mixing salt solution, and the dissolving of principal goods material is controlled at 20% of saturation solubility;
Get the H of Yuan material Chun Du ≧ 99%
2C
2O
4H
2O is 1 liter a oxalic acid solution with per 45.4 gram dose volume, as precipitating reagent.Getting the NaOH of Yuan material Chun Du ≧ 99%, is 1 liter sodium hydroxide solution with per 28.8 gram dose volume, and mixing salt solution and precipitating reagent, sodium hydroxide solution are put into three head tanks;
And stream co-precipitation: under the normal temperature and pressure, open the head tank switch, with 0.2Lmin
-1Flow velocity, under the normal temperature and pressure by conduit with and the mode of stream mixing salt solution and precipitating reagent, NaOH introduced in the batch (-type) mechanical agitation reactor carried out coprecipitation reaction.20 ℃ of reaction temperatures, in 60 minutes reaction time, the sediment ageing time is 16 hours, must mix the oxalate precipitation thing;
With filter paper co-precipitation is filtered, filter cake is taken out spend deionised water then, filter with filter paper, washed twice gets final product;
Co-precipitation sample behind the filtration washing is placed baking oven, be controlled at 70～90 ℃, dry 7 hours;
Decomposition-reduction: the co-precipitation sample after will drying places the decomposition-reduction stove, and atmosphere is general hydrogen, and air speed is 3000h
-1, at first emptying 0.5h heats up afterwards, and in 200 ℃ of constant temperature 2h, 450 ℃ of constant temperature 2.5h, 600 ℃ of constant temperature 2.5h, programming rate are 10 ℃ of min
-1
After decomposition-reduction is finished, sample cooling under general hydrogen protection, general hydrogen air speed 2000h
-1Following passivation, passivation time are 10 hours, and 25 ℃ of temperature are treated to take out sample after passivation is finished from reaction tube.
The yield of metal component Fe, Cu, Ni is respectively 92.7%, 99.7%, 85.9%, places 15 days oxygen content 3.64 ‰ after the passivation.
Example 3
Get the principal goods material FeSO of Yuan material Chun Du ≧ 96%
47H
2The CuSO of O 56 Ke ， ≧ 98%
45H
2The NiSO of O30.6 Ke ， ≧ 98%
46H
2O 10.8 gram is mixed with volume and is 1 liter mixing salt solution, and the dissolving of principal goods material is controlled at 20% of saturation solubility;
Get the H of Yuan material Chun Du ≧ 99%
2C
2O
4H
2O is 1 liter a oxalic acid solution with per 68 gram dose volume, as precipitating reagent.Getting the NaOH of Yuan material Chun Du ≧ 99%, is 1 liter sodium hydroxide solution with per 21.6 gram dose volume, and mixing salt solution and precipitating reagent, sodium hydroxide solution are put into three head tanks;
And stream co-precipitation: under the normal temperature and pressure, open the head tank switch, with 0.2Lmin
-1Flow velocity, under the normal temperature and pressure by conduit with and the mode of stream mixing salt solution and precipitating reagent, NaOH introduced in the batch (-type) mechanical agitation reactor carried out coprecipitation reaction.90 ℃ of reaction temperatures, in 20 minutes reaction time, the sediment ageing time is 16 hours, must mix the oxalate precipitation thing;
With filter paper co-precipitation is filtered, filter cake is taken out spend deionised water then, filter with filter paper, washed twice gets final product;
Co-precipitation sample behind the filtration washing is placed baking oven, be controlled at 70～90 ℃, dry 7 hours;
Decomposition-reduction: the co-precipitation sample after will drying places the decomposition-reduction stove, and atmosphere is general hydrogen, and air speed is 3000h
-1, at first emptying 0.5h heats up afterwards, and in 200 ℃ of constant temperature 2h, 450 ℃ of constant temperature 2.5h, 600 ℃ of constant temperature 2.5h, programming rate are 10 ℃ of min
-1
After decomposition-reduction is finished, sample cooling under general hydrogen protection, general hydrogen air speed 4000h
-1Following passivation, passivation time are 11 hours, and 50 ℃ of temperature are treated to take out sample after passivation is finished from reaction tube.
The yield of metal component Fe, Cu, Ni is respectively 91.3%, 97.4%, 88.2%, places 15 days oxygen content 3.23 ‰ after the passivation.
Example 4
Get the principal goods material FeSO of Yuan material Chun Du ≧ 96%
47H
2The CuSO of O84 Ke ， ≧ 98%
45H
2The NiSO of O38.4 Ke ， ≧ 98%
46H
2O 13.4 gram is mixed with volume and is 1 liter mixing salt solution, and the dissolving of principal goods material is controlled at 30% of saturation solubility;
Get the H of Yuan material Chun Du ≧ 99%
2C
2O
4H
2O is 1 liter a oxalic acid solution with per 63.6 gram dose volume, as precipitating reagent.Getting the NaOH of Yuan material Chun Du ≧ 99%, is 1 liter sodium hydroxide solution with per 60 gram dose volume, and mixing salt solution and precipitating reagent, sodium hydroxide solution are put into three head tanks;
And stream co-precipitation: under the normal temperature and pressure, open the head tank switch, with 0.5Lmin
-1Flow velocity, under the normal temperature and pressure by conduit with and the mode of stream mixing salt solution and precipitating reagent, NaOH introduced in the batch (-type) mechanical agitation reactor carried out coprecipitation reaction.20 ℃ of reaction temperatures, in 80 minutes reaction time, the sediment ageing time is 20 hours, must mix the oxalate precipitation thing;
With filter paper co-precipitation is filtered, filter cake is taken out spend deionised water then, filter with filter paper, washed twice gets final product;
Co-precipitation sample behind the filtration washing is placed baking oven, be controlled at 70～90 ℃, dry 8 hours;
Decomposition-reduction: the co-precipitation sample after will drying places the decomposition-reduction stove, and atmosphere is general hydrogen, and air speed is 3000h
-1, at first emptying 0.5h heats up afterwards, and in 200 ℃ of constant temperature 2.5h, 450 ℃ of constant temperature 3h, 600 ℃ of constant temperature 2.5h, programming rate are 10 ℃ of min
-1
After decomposition-reduction is finished, sample cooling under general hydrogen protection, general hydrogen air speed 3000h
-1Following passivation, passivation time are 4 hours, and 30 ℃ of temperature are treated to take out sample after passivation is finished from reaction tube.
The yield of metal component Fe, Cu, Ni is respectively 95.4%, 99.0%, 93.1%, places 5 days oxygen content 3.04 ‰ after the passivation.
Example 5
Get the principal goods material FeSO of Yuan material Chun Du ≧ 96%
47H
2The CuSO of O84 Ke ， ≧ 98%
45H
2The NiSO of O45.9 Ke ， ≧ 98%
46H
2O16.2 gram is mixed with volume and is 1 liter mixing salt solution, and the dissolving of principal goods material is controlled at 30% of saturation solubility;
Get the H of Yuan material Chun Du ≧ 99%
2C
2O
4H
2O is 1 liter a oxalic acid solution with per 102 gram dose volume, as precipitating reagent.Getting the NaOH of Yuan material Chun Du ≧ 99%, is 1 liter sodium hydroxide solution with per 32.4 gram dose volume, and mixing salt solution and precipitating reagent, sodium hydroxide solution are put into three head tanks;
And stream co-precipitation: under the normal temperature and pressure, open the head tank switch, with 0.4Lmin
-1Flow velocity, under the normal temperature and pressure by conduit with and the mode of stream mixing salt solution and precipitating reagent, NaOH introduced in the batch (-type) mechanical agitation reactor carried out coprecipitation reaction.70 ℃ of reaction temperatures, in 20 minutes reaction time, the sediment ageing time is 20 hours, must mix the oxalate precipitation thing;
With filter paper co-precipitation is filtered, filter cake is taken out spend deionised water then, filter with filter paper, washed twice gets final product;
Co-precipitation sample behind the filtration washing is placed baking oven, be controlled at 70～90 ℃, dry 8 hours;
Decomposition-reduction: the co-precipitation sample after will drying places the decomposition-reduction stove, and atmosphere is general hydrogen, and air speed is 3000h
-1, at first emptying 0.5h heats up afterwards, and in 200 ℃ of constant temperature 2.5h, 450 ℃ of constant temperature 3h, 600 ℃ of constant temperature 2.5h, programming rate are 10 ℃ of min
-1
After decomposition-reduction is finished, sample cooling under general hydrogen protection, general hydrogen air speed 3000h
-1Following passivation, passivation time are 8 hours, and 45 ℃ of temperature are treated to take out sample after passivation is finished from reaction tube.
The yield of metal component Fe, Cu, Ni is respectively 93.5%, 98.7%, 93.7%, places 5 days oxygen content 2.94 ‰ after the passivation.
Example 6
Get the principal goods material FeSO of Yuan material Chun Du ≧ 96%
47H
2The CuSO of O84 Ke ， ≧ 98%
45H
2The NiSO of O45.9 Ke ， ≧ 98%
46H
2O16.2 gram is mixed with volume and is 1 liter mixing salt solution, and the dissolving of principal goods material is controlled at 30% of saturation solubility;
Get the H of Yuan material Chun Du ≧ 99%
2C
2O
4H
2O is 1 liter a oxalic acid solution with per 68 gram dose volume, as precipitating reagent.Getting the NaOH of Yuan material Chun Du ≧ 99%, is 1 liter sodium hydroxide solution with per 43.2 gram dose volume, and mixing salt solution and precipitating reagent, sodium hydroxide solution are put into three head tanks;
And stream co-precipitation: under the normal temperature and pressure, open the head tank switch, with 0.3Lmin
-1Flow velocity, under the normal temperature and pressure by conduit with and the mode of stream mixing salt solution and precipitating reagent, NaOH introduced in the batch (-type) mechanical agitation reactor carried out coprecipitation reaction.90 ℃ of reaction temperatures, in 60 minutes reaction time, the sediment ageing time is 20 hours, must mix the oxalate precipitation thing;
With filter paper co-precipitation is filtered, filter cake is taken out spend deionised water then, filter with filter paper, washed twice gets final product;
Co-precipitation sample behind the filtration washing is placed baking oven, be controlled at 70～90 ℃, dry 8 hours;
Decomposition-reduction: the co-precipitation sample after will drying places the decomposition-reduction stove, and atmosphere is general hydrogen, and air speed is 3000h
-1, at first emptying 0.5h heats up afterwards, and in 200 ℃ of constant temperature 2.5h, 450 ℃ of constant temperature 3h, 600 ℃ of constant temperature 2.5h, programming rate are 10 ℃ of min
-1
After decomposition-reduction is finished, sample cooling under general hydrogen protection, general hydrogen air speed 3000h
-1Following passivation, passivation time are 6 hours, and 100 ℃ of temperature are treated to take out sample after passivation is finished from reaction tube.
The yield of metal component Fe, Cu, Ni is respectively 92.7%, 99.7%, 85.9%, places 5 days oxygen content 2.89 ‰ after the passivation.
Example 7
Get the principal goods material FeSO of Yuan material Chun Du ≧ 96%
47H
2The CuSO of O112 Ke ， ≧ 98%
45H
2The NiSO of O51.2 Ke ， ≧ 98%
46H
2O17.8 gram is mixed with volume and is 1 liter mixing salt solution, and the dissolving of principal goods material is controlled at 40% of saturation solubility;
Get the H of Yuan material Chun Du ≧ 99%
2C
2O
4H
2O is 1 liter a oxalic acid solution with per 84 gram dose volume, as precipitating reagent.Getting the NaOH of Yuan material Chun Du ≧ 99%, is 1 liter sodium hydroxide solution with per 26.7 gram dose volume, and mixing salt solution and precipitating reagent, sodium hydroxide solution are put into three head tanks; And stream co-precipitation: under the normal temperature and pressure, open the head tank switch, with 0.1Lmin
-1Flow velocity, under the normal temperature and pressure by conduit with and the mode of stream mixing salt solution and precipitating reagent, NaOH introduced in the batch (-type) mechanical agitation reactor carried out coprecipitation reaction.20 ℃ of reaction temperatures, in 120 minutes reaction time, the sediment ageing time is 24 hours, must mix the oxalate precipitation thing;
With filter paper co-precipitation is filtered, filter cake is taken out spend deionised water then, filter with filter paper, washed twice gets final product;
Co-precipitation sample behind the filtration washing is placed baking oven, be controlled at 70～90 ℃, dry 10 hours;
Decomposition-reduction: the co-precipitation sample after will drying places the decomposition-reduction stove, and atmosphere is general hydrogen, and air speed is 3000h
-1, at first emptying 0.5h heats up afterwards, and in 200 ℃ of constant temperature 3h, 450 ℃ of constant temperature 3h, 600 ℃ of constant temperature 3h, programming rate are 10 ℃ of min
-1
After decomposition-reduction is finished, sample cooling under general hydrogen protection, general hydrogen air speed 3000h-
1Following passivation, passivation time are 4 hours, and 25 ℃ of temperature are treated to take out sample after passivation is finished from reaction tube.
The yield of metal component Fe, Cu, Ni is respectively 98.7%, 98.9%, 97.8%, places 10 days oxygen content 3.13 ‰ after the passivation.
Example 8
Get the principal goods material FeSO of Yuan material Chun Du ≧ 96%
47H
2The CuSO of O112 Ke ， ≧ 98%
45H
2The NiSO of O61.2 Ke ， ≧ 98%
46H
2O21.6 gram is mixed with volume and is 1 liter mixing salt solution, and the dissolving of principal goods material is controlled at 40% of saturation solubility;
Get the H of Yuan material Chun Du ≧ 99%
2C
2O
4H
2O is 1 liter a oxalic acid solution with per 90.7 gram dose volume, as precipitating reagent.Getting the NaOH of Yuan material Chun Du ≧ 99%, is 1 liter sodium hydroxide solution with per 57.6 gram dose volume, and mixing salt solution and precipitating reagent, sodium hydroxide solution are put into three head tanks;
And stream co-precipitation: under the normal temperature and pressure, open the head tank switch, with 0.2Lmin
-1Flow velocity, under the normal temperature and pressure by conduit with and the mode of stream mixing salt solution and precipitating reagent, NaOH introduced in the batch (-type) mechanical agitation reactor carried out coprecipitation reaction.50 ℃ of reaction temperatures, in 20 minutes reaction time, the sediment ageing time is 24 hours, must mix the oxalate precipitation thing;
With filter paper co-precipitation is filtered, filter cake is taken out spend deionised water then, filter with filter paper, washed twice gets final product;
Co-precipitation sample behind the filtration washing is placed baking oven, be controlled at 70～90 ℃, dry 10 hours;
Decomposition-reduction: the co-precipitation sample after will drying places the decomposition-reduction stove, and atmosphere is general hydrogen, and air speed is 3000h
-1, at first emptying 0.5h heats up afterwards, and in 200 ℃ of constant temperature 3h, 450 ℃ of constant temperature 3h, 600 ℃ of constant temperature 3h, programming rate are 10 ℃ of min
-1
After decomposition-reduction is finished, sample cooling under general hydrogen protection, general hydrogen air speed 3000h
-1Following passivation, passivation time are 2 hours, and 120 ℃ of temperature are treated to take out sample after passivation is finished from reaction tube.
The yield of metal component Fe, Cu, Ni is respectively 98.7%, 98.9%, 97.8%, places 10 days oxygen content 3.06 ‰ after the passivation.
Claims (2)
1. method for preparing diamond metal anchoring agent is characterized in that comprising following processing step:
A. ferrous sulfate, nickelous sulfate and copper sulphate at room temperature are mixed with mixing salt solution in the ratio of 5～6:3:1, the dissolving of principal goods material ferrous sulfate is controlled at 10～40% of saturation solubility;
B. oxalic acid is made precipitating reagent, and its concentration is 1.0～1.5 times of salt-mixture total concentration, and with the pH value of NaOH conditioned reaction system, control method is oxalic acid and naoh concentration 1:1～1:3, and the volume of adding equates;
C. place reactor to carry out equal-volume mixing salt solution and precipitating reagent, sodium hydroxide solution and flow co-precipitation, solution adding speed is 0.1～0.4Lmin
-1, reaction temperature is 20～100 ℃, and the reaction time is 0.3～2 hour, and the sediment ageing time is 12～24 hours, must mix the oxalate precipitation thing;
D. will mix the oxalate precipitation thing and filter, washing, 70～90 ℃ dry 6～10 hours down, heat up hydrogen gas space velocity 3000h at 200～600 ℃ of downstairs
-1, decomposition-reduction 5～11 hours;
E. with the article after the above-mentioned reduction, carry out passivation under general nitrogen atmosphere, general hydrogen air speed is 1000h
-1～4000h
-1, passivation temperature is 10 ℃～200 ℃, passivation time is 2～12 hours, promptly gets product.
2. according to the preparation method of the described diamond metal anchoring agent of claim 1, it is characterized in that: product was placed after 5～15 days, measured its oxygen content with the temperature programmed reduction method and was lower than 4 ‰.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100640651A CN101462172A (en) | 2009-01-13 | 2009-01-13 | Method for preparing diamond metal anchoring agent |
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|---|---|---|---|
| CNA2009100640651A CN101462172A (en) | 2009-01-13 | 2009-01-13 | Method for preparing diamond metal anchoring agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104550932A (en) * | 2014-12-25 | 2015-04-29 | 铜陵市经纬流体科技有限公司 | Iron-based-fused alumina zirconia powder metallurgy valve material and preparation method thereof |
| CN108941535A (en) * | 2018-08-02 | 2018-12-07 | 泉州众志金刚石工具有限公司 | The application and alternative of organic acid nickel substitution nano nickel in diamond matrix |
-
2009
- 2009-01-13 CN CNA2009100640651A patent/CN101462172A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104550932A (en) * | 2014-12-25 | 2015-04-29 | 铜陵市经纬流体科技有限公司 | Iron-based-fused alumina zirconia powder metallurgy valve material and preparation method thereof |
| CN108941535A (en) * | 2018-08-02 | 2018-12-07 | 泉州众志金刚石工具有限公司 | The application and alternative of organic acid nickel substitution nano nickel in diamond matrix |
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