CN105220188B - A kind of preparation method of nickel molybdenum aluminium molybdenum disilicide composite deposite - Google Patents
A kind of preparation method of nickel molybdenum aluminium molybdenum disilicide composite deposite Download PDFInfo
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- CN105220188B CN105220188B CN201510643414.0A CN201510643414A CN105220188B CN 105220188 B CN105220188 B CN 105220188B CN 201510643414 A CN201510643414 A CN 201510643414A CN 105220188 B CN105220188 B CN 105220188B
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Abstract
A kind of preparation method of nickel molybdenum aluminium molybdenum disilicide composite deposite of the present invention, molybdenum disilicide particulate is carried out pickling, washing, dried by one；Nickel salt, molybdenum compound, aluminium salt, complexing agent, chloride are weighed, is dissolved after mixing with water, regulation solution ph is 7.3~9.7, and nickel salt molybdenum compound aluminium salt complexing agent chloride mixed liquor is made；Molybdenum disilicide particulate, first nickel salt molybdenum compound aluminium salt complexing agent chloride mixed liquor are mixed with surfactant, second batch nickel salt molybdenum compound aluminium salt complexing agent chloride mixed liquor is added after grinding, electroplate liquid is made in stirring, plating piece to be plated is put into electroplate liquid and electroplated, anode is nickel, and negative electrode is nickel alloy to be electroplated, after plating is finished, plating piece is rinsed with water, is air-dried and is obtained nickel molybdenum aluminium molybdenum disilicide composite deposite.It is respectively 2.5~9.2% and 1.2~6.5% to determine nickel molybdenum aluminium molybdenum disilicide composite medium aluminium and silicone content using energy disperse spectroscopy.
Description
Technical field
The invention belongs to chemical field, it is related to a kind of hot coating technology, specifically a kind of nickel molybdenum aluminium-molybdenum disilicide is multiple
Close the preparation method of coating.
Background technology
The practicable method for increasing substantially aero-engine operating temperature at present is to use Thermal Barrier Coating Technologies.Obtain
The thermal barrier coating of practical application is mostly double-decker, ceramic layer due to it is heat-insulated, anticorrosive, wash away and erosion performance,
It is used as the top layer of thermal barrier coating.Because the thermal coefficient of expansion of ceramics and high-temperature structural material is mismatched, it is necessary to play high temperature resistance oxygen
Change corrosion and improve matrix and the metal bonding coating of the effect of ceramic coating physical compatibility, metal bonding coating is bottom.At present
A kind of bonding layer material that thermal barrier coating is generally used is MCrAlY (M：Ni, Co or Ni+Co).We have studied nickel molybdenum coating,
Nickel molybdenum rare coating, nickel molybdenum-molybdenum disilicide composite deposite, nickel molybdenum rare-molybdenum disilicide composite deposite, nickel molybdenum aluminium coat, nickel molybdenum
Aluminium is rare earth coated to be used as tack coat.Appropriate molybdenum disilicide is added in nickel molybdenum aluminium coat, the high temperature resistance oxygen of tack coat can be improved
Change corrosivity, but the report still without nickel molybdenum aluminium-molybdenum disilicide composite deposite practical application at present.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of nickel molybdenum aluminium-molybdenum disilicide composite deposite
Preparation method, the preparation method of described this nickel molybdenum aluminium-molybdenum disilicide composite deposite solves bonding of the prior art
The not good technical problem of the effect of layer material high temperature oxidation corrosion resistance.
A kind of preparation method of nickel molybdenum aluminium-molybdenum disilicide composite deposite of the present invention, comprises the following steps：
（1）Particle diameter is carried out pickling, washing, the step dried by one for 10 μm~10nm molybdenum disilicide particulate；
（2）Nickel salt, molybdenum compound, aluminium salt, complexing agent, chloride are weighed, after mixing, is dissolved with water so that nickel salt, molybdenum
Compound, aluminium salt, complexing agent, the concentration of chloride be respectively 9 ~ 405g/L, 9 ~ 805g/L, 9 ~ 355g/L, 4 ~ 105g/L, 9 ~
305g/L, is 7.3~9.7 with aqueous slkali regulation solution ph, nickel salt-molybdenum compound-aluminium salt-complexing agent-chloride is made and mixes
Close liquid；
Wherein nickel salt is the mixture of one or both of nickel nitrate, nickel chloride or nickel sulfate composition described above；Molybdenum
Compound is the mixture of one or both of ammonium molybdate, molybdenum pentachloride, ammonium phosphomolybdate or sodium molybdate composition described above；Aluminium salt
The mixture constituted for one or both of aluminum sulfate or alchlor, complexing agent is hydroxyacetic acid, amion acetic acid, lemon
A kind of and more than one complexing agent mixture in lemon acid, oxalic acid, lactic acid, malic acid, succinic acid or tartaric acid, chlorination
Thing is a kind of and more than one the chloride mix in ammonium chloride, sodium chloride or potassium chloride；
（3）By step（1）The molybdenum disilicide particulate of preparation, first nickel salt-molybdenum compound-aluminium salt-complexing agent-chloride
Mixed liquor is mixed with surfactant, first nickel salt-molybdenum compound-aluminium salt-complexing agent-chloride mixed liquor and molybdenum disilicide
Volume mass ratio be 1~2 ml:It is transferred to after 1g, grinding in another container and continues to add second batch nickel salt-molybdenum compound-
Aluminium salt-complexing agent-chloride mixed liquor so that the concentration of molybdenum disilicide is 3~60g/L, the ultimate density of surfactant is
0.009~0.95g/L, and the h of mechanical agitation 4~12 under the conditions of rotating speed is 300~900rpm, are made electroplate liquid, wherein, table
Face activating agent is selected from triton x-100, neopelex, cetyl trimethylammonium bromide, hexadecyl pyrrole
One or more kinds of mixtures in pyridine or Macrogol 6000；
（4）Plating piece to be plated is put into electroplate liquid and electroplated, anode is nickel, negative electrode is nickel alloy to be electroplated, the work of plating
Skill condition is that 500~5000Hz of pulse frequency, dutycycle are 0.4~0.9,10~25A/dm of current density2, bath pH values
7.3~9.7,30~60 DEG C of electroplating temperature, 100~600rpm of speed of agitator, 10~60min of electroplating time, after plating is finished, plating
Part is rinsed with water, is air-dried and has been obtained nickel molybdenum aluminium-molybdenum disilicide composite deposite.
Further, in step 1）In, particle diameter is first cleaned for 10 μm~10nm molybdenum disilicide particulate with acetone, then soaks
0.2~1h in 1~6mol/L hydrochloric acid solution is steeped, suction filtration is washed to neutrality, 0.5~5h is dried at 50~100 DEG C.
Further, described aqueous slkali is sodium carbonate liquor, and its mass percent concentration is 5 ~ 20%.
Using Bruker AXS Microanalysis GmbH energy disperse spectroscopies determine nickel molybdenum aluminium-molybdenum disilicide composite medium aluminium and
Silicone content is respectively 2.5~9.2% and 1.2~6.5%.
Embodiment
Embodiment 1
It is 10 μm of molybdenum disilicide particulate 3g in 100mL beaker to weigh particle diameter, plus 5mL acetone, stirs 5min, suction filtration,
By molybdenum disilicide particulate in 50mL beaker, plus 6mol ﹒ L-1Hydrochloric acid solution 5mL, soaks 0.2h, and suction filtration is washed to neutrality,
5h is dried in 50 DEG C of baking ovens.5g nickel nitrates, 4g nickel sulfates, 9g ammonium molybdates, 9g aluminum sulfate, 2g hydroxyl second are added in 2L beaker
Acid, 2g citric acids, 9g ammonium chlorides, plus 985mL water dissolve to form nickel nitrate-nickel sulfate-ammonium molybdate-aluminum sulfate-hydroxyacetic acid-lemon
Lemon acid-ammonium chloride mixed solution, is 7.3 with sodium carbonate liquor regulation solution ph, moves into 1L volumetric flasks, be diluted with water to quarter
Degree.By the molybdenum disilicide particulate of above-mentioned processing in mortar, plus 0.009g Macrogol 6000s surfactant, 6mL is above-mentioned matches somebody with somebody
Nickel nitrate-nickel sulfate-ammonium molybdate-aluminum sulfate-hydroxyacetic acid-citric acid-ammonium chloride mixed liquor of system, grinds 30 min, is transferred to
In 2L beaker, nickel nitrate-nickel sulfate-ammonium molybdate-aluminum sulfate-hydroxyacetic acid-citric acid-chlorine of the above-mentioned preparations of 994mL is added
Change ammonium mixed liquor, mechanical agitation, speed of agitator is 300rpm, and mixing time is 12 h, and electroplate liquid is made.By 80mm × 80mm ×
0.5mm's treats that nickel plating alloy plate is put into electroplate liquid and for negative electrode, and anode is 150mm × 100mm × 2mm sheet nickel, magnetic
Power is stirred, and speed of agitator is 100rpm, and current density is 10A/dm2, bath pH values are 7.3, and temperature is 30 DEG C, plating time
For 60min.Plating piece is taken out, rinses net with water, air-dries.Determined using Bruker AXS Microanalysis GmbH energy disperse spectroscopies
The content of aluminium and silicon is respectively 2.5% and 1.2% in nickel molybdenum aluminium-molybdenum disilicide coating.
Embodiment 2
It is 10nm molybdenum disilicide particulate 60g in 200mL beaker to weigh particle diameter, plus 100mL acetone stirs 5min, taken out
Filter, by molybdenum disilicide particulate in 200mL beaker, plus 1mol ﹒ L-1Hydrochloric acid solution 100mL, soaks 1h, suction filtration, in being washed to
Property, 0.5h is dried in 100 DEG C of baking ovens.Added in 2L beaker 205g nickel chlorides, 200g nickel nitrates, 805g sodium molybdates,
150g alchlors, 205g aluminum sulfate, 30g amion acetic acids, 75g oxalic acid, 305g sodium chloride, plus 985mL water dissolve to form chlorination
Nickel-nickel nitrate-sodium molybdate-alchlor-aluminum sulfate-amion acetic acid-oxalic acid-sodium chloride mixed solution, is adjusted with sodium carbonate liquor
It is 9.7 to save solution ph, moves into 1L volumetric flasks, is diluted with water to scale.By the molybdenum disilicide particulate of above-mentioned processing in mortar
In, plus 0.45g brocides and 0.5g triton x-100s surfactant, nickel chloride-nitre of the above-mentioned preparations of 60mL
Sour sodium-alchlor-aluminum sulfate-amion acetic acid-oxalic acid-sodium chloride the mixed liquor of sour nickel-molybdenum, grinds 30 min, is transferred to 2L burning
In cup, nickel chloride-nickel nitrate-sodium molybdate-alchlor-aluminum sulfate-amion acetic acid-oxalic acid-chlorine of the above-mentioned preparations of 940mL is added
Change sodium mixed liquor, mechanical agitation, speed of agitator is 900rpm, and mixing time is 4h, electroplate liquid is made.By 80mm × 80mm ×
0.5mm's treats that nickel plating alloy plate is put into electroplate liquid and for negative electrode, and anode is 150mm × 100mm × 2mm sheet nickel, magnetic
Power is stirred, and speed of agitator is 600rpm, and current density is 25A/dm2, bath pH values are 9.7, and temperature is 60 DEG C, plating time
For 10min.Plating piece is taken out, rinses net with water, air-dries.Determined using Bruker AXS Microanalysis GmbH energy disperse spectroscopies
The content of aluminium and silicon is respectively 9.2% and 6.5% in nickel molybdenum aluminium-molybdenum disilicide coating.
Embodiment 3
It is 5 μm of molybdenum disilicide particulate 30g in 100mL beaker to weigh particle diameter, plus 50mL acetone, stirs 5min, suction filtration,
By molybdenum disilicide particulate in 100mL beaker, plus 3mol ﹒ L-1Hydrochloric acid solution 50mL, soaks 0.6h, and suction filtration is washed to neutrality,
3h is dried in 75 DEG C of baking ovens.203g nickel nitrates, 200g molybdenum pentachlorides, 203g ammonium phosphomolybdates, 178g are added in 2L beaker
Alchlor, 10g lactic acid, 10g malic acid, 10g succinic acid, 23g tartaric acid, 53g potassium chloride, 100g ammonium chlorides, plus 985mL water
Dissolving forms nickel nitrate-molybdenum pentachloride-ammonium phosphomolybdate-alchlor-lactic acid-malic acid-succinic acid-tartaric acid-potassium chloride-chlorine
Change ammonium mixed solution, be 8.3 with sodium carbonate liquor regulation solution ph, move into 1L volumetric flasks, be diluted with water to scale.Will be upper
The molybdenum disilicide particulate of processing is stated in mortar, plus 0.4g cetyl trimethylammonium bromides and 0.08g DBSAs
Nickel nitrate-molybdenum pentachloride-ammonium phosphomolybdate-alchlor-lactic acid-malic acid-fourth two of the above-mentioned preparation of natrium surfactant, 45mL
Acid-tartaric acid-potassium chloride-ammonium chloride mixed liquor, grinds 30 min, is transferred in 2L beaker, adds the nitre of the above-mentioned preparations of 955mL
Sour nickel-molybdenum pentachloride-ammonium phosphomolybdate-alchlor-lactic acid-malic acid-succinic acid-tartaric acid-potassium chloride-ammonium chloride mixing
Liquid, mechanical agitation, speed of agitator is 600rpm, and mixing time is 8h, and electroplate liquid is made.By treating for 80mm × 80mm × 0.5mm
Nickel plating alloy plate is put into electroplate liquid and is negative electrode, and anode is 150mm × 100mm × 2mm sheet nickel, and magnetic agitation is stirred
Mix rotating speed is 350rpm, and current density is 17.5A/dm2, bath pH values are 8.3, and temperature is 45 DEG C, and plating time is
45min.Plating piece is taken out, rinses net with water, air-dries.Nickel is determined using Bruker AXS Microanalysis GmbH energy disperse spectroscopies
The content of aluminium and silicon is respectively 7.9% and 4.2% in molybdenum aluminium-molybdenum disilicide coating.
Claims (1)
1. a kind of preparation method of nickel molybdenum aluminium-molybdenum disilicide composite deposite, it is characterised in that comprise the following steps：
（1）Particle diameter is carried out pickling, washing, the step dried by one for 10 μm~10nm molybdenum disilicide particulate；It is by particle diameter
10 μm~10nm molybdenum disilicide particulate is first cleaned with acetone, then is soaked in 0.2~1h in 1~6mol/L hydrochloric acid solution, is taken out
Filter, is washed to neutrality, and 0.5~5h is dried at 50~100 DEG C；
（2）Weigh nickel salt, molybdenum compound, aluminium salt, complexing agent, chloride to be added in a reaction vessel, after mixing, with water-soluble
Solution so that nickel salt, molybdenum compound, aluminium salt, complexing agent, the concentration of chloride are respectively 9 ~ 405g/L, 9 ~ 805g/L, 9 ~ 355g/
L, 4 ~ 105g/L, 9 ~ 305g/L, are 7.3~9.7 with aqueous slkali regulation solution ph, described aqueous slkali is sodium carbonate liquor,
Its mass percent concentration is 5 ~ 20%；Nickel salt-molybdenum compound-aluminium salt-complexing agent-chloride mixed liquor is made；
Wherein nickel salt is the mixture of one or both of nickel nitrate, nickel chloride or nickel sulfate composition described above；Molybdenum compound
For the mixture of one or both of ammonium molybdate, molybdenum pentachloride, ammonium phosphomolybdate or sodium molybdate composition described above；Aluminium salt is sulphur
One or both of sour aluminium or alchlor composition mixture, complexing agent be hydroxyacetic acid, amion acetic acid, citric acid,
A kind of and more than one complexing agent mixture in oxalic acid, lactic acid, malic acid, succinic acid or tartaric acid, chloride is chlorine
Change a kind of and more than one the chloride mix in ammonium, sodium chloride or potassium chloride；
（3）By step（1）The molybdenum disilicide particulate of preparation, first nickel salt-molybdenum compound-aluminium salt-complexing agent-chloride mixing
Liquid is mixed with surfactant, the body of first nickel salt-molybdenum compound-aluminium salt-complexing agent-chloride mixed liquor and molybdenum disilicide
Product mass ratio is 1~2 ml:It is transferred to after 1g, grinding in another container and adds second batch nickel salt-molybdenum compound-aluminium salt-network
Mixture-chloride mixed liquor so that the concentration of molybdenum disilicide is 3~60g/L, the ultimate density of surfactant for 0.009~
0.95g/L, and the h of mechanical agitation 4~12 under the conditions of rotating speed is 300~900rpm, are made electroplate liquid, wherein, surfactant
Selected from triton x-100, neopelex, cetyl trimethylammonium bromide, brocide or poly-
One or more kinds of mixtures in ethylene glycol 6000；
（4）Plating piece to be plated is put into electroplate liquid and electroplated, anode is nickel, negative electrode is nickel alloy to be electroplated, electroplating technique bar
Part is that 500~5000Hz of pulse frequency, dutycycle are 0.4~0.9,10~25A/dm of current density2, bath pH values 7.3~
9.7,30~60 DEG C of electroplating temperature, 100~600rpm of speed of agitator, 10~60min of electroplating time, after plating is finished, plating piece is used
Water is rinsed, and is air-dried and has been obtained nickel molybdenum aluminium-molybdenum disilicide composite deposite.
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| US6776891B2 (en) * | 2001-05-18 | 2004-08-17 | Headway Technologies, Inc. | Method of manufacturing an ultra high saturation moment soft magnetic thin film |
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|---|---|---|---|---|
| CN102908909A (en) * | 2012-11-13 | 2013-02-06 | 上海应用技术学院 | Nickel-copper-rare earth-aluminum oxide catalysis separation composite film and preparation method and application thereof |
| CN103436924A (en) * | 2013-08-12 | 2013-12-11 | 上海应用技术学院 | Electroplating liquid used for forming nickel molybdenum-molybdenum disilicide composite plating, and preparation method and application of electroplating liquid |
| CN104278301A (en) * | 2014-10-23 | 2015-01-14 | 上海应用技术学院 | Nickel-molybdenum-aluminium coating and preparation method thereof |
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