CN104892006B - A kind of phosphate doped ceramics coating material and preparation method thereof - Google Patents
A kind of phosphate doped ceramics coating material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of phosphate doped ceramics coating material; the problem of being easily lost under the impact of high speed dust and damp and hot, corrosive environment the present invention is to solve metal material; by in metal material surface applying phosphate doped ceramics material; so as to have certain protective effect to metal material, reach the purpose for extending metal material service life.Phosphate doped ceramics material is made up of aluminium dihydrogen phosphate biphosphate chromium solution, diluent and ceramic composition three parts, and preparation process is as follows：First, aluminium dihydrogen phosphate biphosphate chromium solution is prepared；2nd, diluent is prepared；3rd, ceramic composition is prepared；4th, phosphate doped ceramics coating material is prepared.Phosphate doped ceramics coating material prepared by the present invention, wear-resisting, corrosion-resistant, resistance to elevated temperatures is good, and have certain adhesive property, the gas erosion shield of material can be glued by being mainly used in metal material and other.
Description
Technical field
The present invention relates to ceramic coated materials technical field, more particularly to a kind of phosphate doped ceramics coating material and its
Preparation method, be mainly used in pipeline in metallurgy, electric power, coal industry, burning between part it is wear-resisting, corrosion-resistant and resistant to elevated temperatures
Protection.
Background technology
With the development of industrial technology, the industry such as metallurgy, electric power, coal also improves constantly to the demand of dynamical system；And
And coal supply anxiety and coal dust quality decline, therefore to ensure that operating efficiency then needs to increase the amount of delivering coal of unit interval, this meeting
Make the ash content that is mingled with thermal current coal dust more, air-flow velocity can faster, in addition produce water and nitrogenous, sulfur-bearing, contain after coal combustion
The corrosive gas such as chlorine, these will all cause metallic conduit, burning between etc. part for a long time the impact of high speed dust, high temperature, humidity,
Worked under corrosive environment, accelerate the deterioration of material, the problems such as trigger booster, shut down, cause waste and the time of material
Loss, or even the safety of life-threatening, property.
Therefore design a kind of wear-resisting, corrosion-resistant, resistant to elevated temperatures phosphate doped ceramics material and be coated in metal material surface,
The impact of the direct contact corrosion gas of metal and high speed dust can be effectively protected, so as to extend the service life of material.
The content of the invention
The present invention be in order to solve metal material high speed dust impact and damp and hot, corrosive environment under be easily lost ask
Topic, and a kind of phosphate doped ceramics coating material and preparation method thereof is provided, by coating phosphoric acid in metal material surface
Salt dopping ceramic material, so as to have certain protective effect to metal material, reach the mesh for extending metal material service life
's.
The present invention adopts the following technical scheme that：
The present invention phosphate doped ceramics coating material be by aluminium dihydrogen phosphate-biphosphate chromium solution, diluent and
Ceramic composition forms, and its specific parts by weight composition is as follows：
Aluminium dihydrogen phosphate -1~4 part of biphosphate chromium solution
15~20 parts of diluent
20~40 parts of ceramic composition.
Described aluminium dihydrogen phosphate-biphosphate chromium solution is made up of the raw material of following parts by weight：
The preparation method of described aluminium dihydrogen phosphate-biphosphate chromium solution is as follows：
The phosphoric acid solution that mass fraction is 85%, aluminium hydroxide, potassium bichromate or three oxidations are weighed according to quality parts ratio
Chromium, it is mixed evenly to obtain mixed solution, mixed solution is warming up to 120 DEG C~150 DEG C holding 1h~4h, heating rate is
15 DEG C/min~30 DEG C/min, 15 DEG C~25 DEG C are cooled to after the completion of reaction, the hydrogen peroxide or formaldehyde of formula ratio are added dropwise thereto
And be sufficiently stirred, 15 DEG C~25 DEG C are cooled to after being added dropwise to complete, the acetone or alcohol for then adding formula ratio stirs, and obtains
Aluminium dihydrogen phosphate-biphosphate chromium mixed solution.
Described diluent is made up of the raw material of following parts by weight：
Mass fraction is 85% 80~120 parts of phosphoric acid solution
50~80 parts of distilled water.
The preparation method of described diluent is as follows：
The phosphoric acid solution that mass fraction is 85% is weighed according to quality parts ratio, distilled water, is mixed evenly, obtains dilute
Release agent.
Described ceramic composition is made up of the raw material of following parts by weight：
Wherein, the particle size range of aluminum oxide is 20 μm~200 μm；The particle size range of aluminium nitride is 200nm~1000nm；Stone
The particle size range of English powder is 5 μm~50 μm；The particle size range of lithium feldspar powder is 5 μm~50 μm；The particle size range of zirconium oxide is
300nm~1000nm.
Wherein aluminum oxide, aluminium nitride, silica flour, zirconium oxide, the particle diameter of lithium feldspar powder are required in particle size range, particle diameter
Crossing conference causes coating material uneven；Calcium oxide, in control range, quality can excessively cause to be applicable magnesia quality requirement
Phase shortens；In control range, quality can excessively cause resistance to height for lead orthoplumbate, sodium tetraborate, sodium tripolyphosphate quality requirement
Warm degradation.
The preparation method of described ceramic composition is as follows：
Aluminum oxide, aluminium nitride, zirconium oxide, silica flour, lithium feldspar powder, calcium oxide, magnesia, four oxidations three are weighed by proportioning
Lead, sodium tetraborate and sodium tripolyphosphate, with V-type batch mixer mixing 6h, obtain ceramic composition.
The preparation method of the phosphate doped ceramics coating material of the present invention comprises the following steps that：
(1) aluminium dihydrogen phosphate-biphosphate chromium solution is weighed by proportioning, diluent, be mixed evenly, it is rear to add proportioning
The ceramic composition of amount, uniform muddy is mixed into, obtains phosphate doped ceramics coating material；
(2) the phosphate doped ceramics material that step (1) obtains coated on metal material or can be glued into material surface, controlled
For temperature according to 50 DEG C~150 DEG C, gradient increased temperature, time range is 12h~48h, is molded phosphate doped ceramics material hardening.
In step (2), gradient increased temperature requires that gradient temperature scope is no more than 30 DEG C.Heating up too fast can cause material internal hole
Gap increases, and the heating-up time will require that the heating-up time is short will to cause material hardening not exclusively to fail according to heating.
The positive effect of the present invention is as follows：
The present invention is using alumina-zirconia-silica flour ceramic powder as matrix, wherein the zirconium oxide added is with stronger
Anti-wear performance, aluminium nitride, calcium oxide, magnesia can improve aluminium dihydrogen phosphate-biphosphate chromium solution hardened forming speed
Degree, reduces the forming temperature of material, other powder are capable of the pH value of regulation system, and play a part of sintering aid, silica flour
And the addition of lithium feldspar can reduce the cost of material, aluminium dihydrogen phosphate-biphosphate chromium solution and aluminum oxide, aluminium nitride in addition
For inorganic adhesive component, preferable adhesive property is provided for phosphate doped ceramics material, and it is ceramic high temperature resistant itself, resistance to
Corrosive power is stronger, therefore the phosphate doped ceramics material prepared has wear-resisting, corrosion-resistant, high temperature resistant, cementability strong etc.
Feature.
Embodiment
The following examples are that the present invention is described in further detail.
Embodiment 1：
First, phosphatase 11 00g, the potassium bichromate 2g for weighing mass fraction 85% are added in 500mL there-necked flasks, by mixed solution
It is warming up to 50 DEG C, and 30min is stirred with 500~800r/min speed, to form crocus molten until potassium bichromate is completely dissolved
Liquid；Orange solution is warming up to 70 DEG C, 20g aluminium hydroxides is weighed and is divided into 10 parts, 1 part is added simultaneously every 10min
It is stirred continuously, continues to stir 30min after all adding, be completely dissolved to aluminium hydroxide；Then solution is warming up to 140 DEG C, after
Continuous reaction 1.5h is simultaneously stirred continuously, and is cooled to room temperature after completion of the reaction；10g hydrogen peroxide is weighed again to be added dropwise wherein and constantly stir
Mix, room temperature is cooled to after being added dropwise；Add 10mL acetone solns to stir, aluminium dihydrogen phosphate-biphosphate chromium is made
Solution；
2nd, the phosphoric acid solution 100g and distilled water 70g of mass fraction 85% are weighed, phosphoric acid solution is mixed with distilled water and stirred
Mix uniformly, obtain diluent；
3rd, aluminum oxide 15g, zirconium oxide 12.5g, silica flour 10g, aluminium nitride 0.5g, calcium oxide 0.5g, magnesia are weighed
0.25g, lead orthoplumbate 1g, sodium tetraborate 0.4g, sodium tripolyphosphate 0.4g, lithium feldspar 5g mix powder input V-type batch mixer
6h is closed, obtains ceramic composition；
4th, aluminium dihydrogen phosphate-biphosphate chromium solution 4g, diluent 16g, the ceramic composition obtained in one, two, three is weighed
20g is mixed into uniform muddy, obtains phosphate doped ceramics coating material.
The working life of phosphate doped ceramics coating material：30min~120min.
The curing condition of phosphate doped ceramics material：Phosphate doped ceramics material coated on metal material or can be glued
Material surface surface, 50 DEG C of heating 4h, 70 DEG C of heating 4h, 90 DEG C of heating 8h, 130 DEG C of heating 4h, 150 DEG C of heating 6h, you can make
Phosphate doped ceramics material hardening.
The phosphate doped ceramics material prepared according to above-mentioned technique, is warming up to 1200 DEG C, applies 50N to its surface
Power, material integrally keeps complete and surface without collapsing.It is warming up to 1000 DEG C and tests the heat mistake of phosphate doped ceramics material
Weight situation, as a result thermal weight loss rate is 6.5%；45# steel test piece is bonded, according to " GB/T 7124-2008, adhesive tensile shear
The measure (rigid material is to rigid material) of intensity ", normal temperature shear strength are 3.07MPa, and shear strength is after 500 DEG C of processing 1h
1.76MPa；Stainless steel and phosphate doped ceramics material are used according to " the natural ornamental stone test methods of GB/T 9966.4-2001 "
Material applies 25N pressure, rotating speed 50rpm/min, abrasion loss 0.26g/cm to mill2。
Embodiment 2：
First, phosphatase 11 00g, the potassium bichromate 2g for weighing mass fraction 85% are added in 500mL there-necked flasks, by mixed solution
It is warming up to 50 DEG C, and 30min is stirred with 500~800r/min speed, to form crocus molten until potassium bichromate is completely dissolved
Liquid；Orange solution is warming up to 70 DEG C, 20g aluminium hydroxides is weighed and is divided into 10 parts, 1 part is added simultaneously every 10min
It is stirred continuously, continues to stir 30min after all adding, be completely dissolved to aluminium hydroxide；Then solution is warming up to 140 DEG C, after
Continuous reaction 1.5h is simultaneously stirred continuously, and is cooled to room temperature after completion of the reaction；10g hydrogen peroxide is weighed again to be added dropwise wherein and constantly stir
Mix, room temperature is cooled to after being added dropwise；Add 10mL acetone solns to stir, aluminium dihydrogen phosphate-biphosphate chromium is made
Solution；
2nd, the phosphoric acid solution 100g and distilled water 70g of mass fraction 85% are weighed, phosphoric acid solution is mixed with distilled water and stirred
Mix uniformly, obtain diluent；
3rd, aluminum oxide 15g, zirconium oxide 12.5g, silica flour 10g, aluminium nitride 1g, calcium oxide 1g, magnesia 0.5g are weighed,
Powder is put into V-type batch mixer mixing 6h by lead orthoplumbate 1g, sodium tetraborate 0.4g, sodium tripolyphosphate 0.4g, lithium feldspar 5g, is obtained
To ceramic composition；
4th, aluminium dihydrogen phosphate-biphosphate chromium solution 4g, diluent 16g, the ceramic composition obtained in one, two, three is weighed
20g is mixed into uniform muddy, obtains phosphate doped ceramics coating material.
The working life of phosphate doped ceramics coating material：20min~60min.
The curing condition of phosphate doped ceramics material：Phosphate doped ceramics material coated on metal material or can be glued
Material surface surface, 50 DEG C of heating 3h, 70 DEG C of heating 3h, 90 DEG C of heating 6h, 130 DEG C of heating 3h, 150 DEG C of heating 6h, you can make
Phosphate doped ceramics material hardening.
The phosphate doped ceramics material prepared according to above-mentioned technique, is warming up to 1200 DEG C, applies 50N to its surface
Power, material integrally keeps complete and surface without collapsing.It is warming up to 1000 DEG C and tests the heat mistake of phosphate doped ceramics material
Weight situation, as a result thermal weight loss rate is 8.0%；45# steel test piece is bonded, according to " GB/T 7124-2008, adhesive tensile shear
The measure (rigid material is to rigid material) of intensity ", normal temperature shear strength are 2.54MPa, and shear strength is after 500 DEG C of processing 1h
1.41MPa；Stainless steel and phosphate doped ceramics material are used according to " the natural ornamental stone test methods of GB/T 9966.4-2001 "
Material applies 25N pressure, rotating speed 50rpm/min, abrasion loss 0.32g/cm to mill2。
Embodiment 3：
First, phosphatase 11 00g, the potassium bichromate 2g for weighing mass fraction 85% are added in 500mL there-necked flasks, by mixed solution
It is warming up to 50 DEG C, and 30min is stirred with 500~800r/min speed, to form crocus molten until potassium bichromate is completely dissolved
Liquid；Orange solution is warming up to 70 DEG C, 20g aluminium hydroxides is weighed and is divided into 10 parts, 1 part is added simultaneously every 10min
It is stirred continuously, continues to stir 30min after all adding, be completely dissolved to aluminium hydroxide；Then solution is warming up to 140 DEG C, after
Continuous reaction 1.5h is simultaneously stirred continuously, and is cooled to room temperature after completion of the reaction；10g hydrogen peroxide is weighed again to be added dropwise wherein and constantly stir
Mix, room temperature is cooled to after being added dropwise；Add 10mL acetone solns to stir, aluminium dihydrogen phosphate-biphosphate chromium is made
Solution；
2nd, the phosphoric acid solution 100g and distilled water 70g of mass fraction 85% are weighed, phosphoric acid solution is mixed with distilled water and stirred
Mix uniformly, obtain diluent；
3rd, aluminum oxide 15g, zirconium oxide 12.5g, silica flour 10g, aluminium nitride 0.5g, calcium oxide 0.5g, magnesia are weighed
0.25g, lead orthoplumbate 1g, sodium tetraborate 0.4g, sodium tripolyphosphate 0.4g, lithium feldspar 5g mix powder input V-type batch mixer
6h is closed, obtains ceramic composition；
4th, aluminium dihydrogen phosphate-biphosphate chromium solution 4g, diluent 16g, the ceramic composition obtained in one, two, three is weighed
30g is mixed into uniform muddy, obtains phosphate doped ceramics coating material.
The working life of phosphate doped ceramics coating material：30min~120min.
The curing condition of phosphate doped ceramics material：Phosphate doped ceramics material coated on metal material or can be glued
Material surface surface, 50 DEG C of heating 4h, 70 DEG C of heating 4h, 90 DEG C of heating 8h, 130 DEG C of heating 4h, 150 DEG C of heating 6h, you can make
Phosphate doped ceramics material hardening.
The phosphate doped ceramics material prepared according to above-mentioned technique, is warming up to 1200 DEG C, applies 50N to its surface
Power, material integrally keeps complete and surface without collapsing.It is warming up to 1000 DEG C and tests the heat mistake of phosphate doped ceramics material
Weight situation, as a result thermal weight loss rate is 5.4%；45# steel test piece is bonded, according to " GB/T 7124-2008, adhesive tensile shear
The measure (rigid material is to rigid material) of intensity ", normal temperature shear strength are 3.43MPa, and shear strength is after 500 DEG C of processing 1h
2.06MPa；Stainless steel and phosphate doped ceramics material are used according to " the natural ornamental stone test methods of GB/T 9966.4-2001 "
Material applies 25N pressure, rotating speed 50rpm/min, abrasion loss 0.17g/cm to mill2。
Embodiment 4：
First, phosphatase 11 00g, the potassium bichromate 2g for weighing mass fraction 85% are added in 500mL there-necked flasks, by mixed solution
It is warming up to 50 DEG C, and 30min is stirred with 500~800r/min speed, to form crocus molten until potassium bichromate is completely dissolved
Liquid；Orange solution is warming up to 70 DEG C, 20g aluminium hydroxides is weighed and is divided into 10 parts, 1 part is added simultaneously every 10min
It is stirred continuously, continues to stir 30min after all adding, be completely dissolved to aluminium hydroxide；Then solution is warming up to 140 DEG C, after
Continuous reaction 1.5h is simultaneously stirred continuously, and is cooled to room temperature after completion of the reaction；10g hydrogen peroxide is weighed again to be added dropwise wherein and constantly stir
Mix, room temperature is cooled to after being added dropwise；Add 10mL acetone solns to stir, aluminium dihydrogen phosphate-biphosphate chromium is made
Solution；
2nd, the phosphoric acid solution 100g and distilled water 70g of mass fraction 85% are weighed, phosphoric acid solution is mixed with distilled water and stirred
Mix uniformly, obtain diluent；
3rd, aluminum oxide 15g, zirconium oxide 12.5g, silica flour 10g, aluminium nitride 0.5g, calcium oxide 0.5g, magnesia are weighed
0.25g, lead orthoplumbate 1g, sodium tetraborate 0.4g, sodium tripolyphosphate 0.4g, lithium feldspar 5g mix powder input V-type batch mixer
6h is closed, obtains ceramic composition；
4th, aluminium dihydrogen phosphate-biphosphate chromium solution 8g, diluent 12g, the ceramic composition obtained in one, two, three is weighed
20g is mixed into uniform muddy, obtains phosphate doped ceramics coating material.
The working life of phosphate doped ceramics coating material：30min~90min.
The curing condition of phosphate doped ceramics material：Phosphate doped ceramics material coated on metal material or can be glued
Material surface surface, 50 DEG C of heating 6h, 70 DEG C of heating 6h, 90 DEG C of heating 12h, 130 DEG C of heating 6h, 150 DEG C of heating 8h, you can make
Phosphate doped ceramics material hardening.
The phosphate doped ceramics material prepared according to above-mentioned technique, is warming up to 1200 DEG C, applies 50N to its surface
Power, material integrally keeps complete and surface without collapsing.It is warming up to 1000 DEG C and tests the heat mistake of phosphate doped ceramics material
Weight situation, as a result thermal weight loss rate is 5.7%；45# steel test piece is bonded, according to " GB/T 7124-2008, adhesive tensile shear
The measure (rigid material is to rigid material) of intensity ", normal temperature shear strength are 3.50MPa, and shear strength is after 500 DEG C of processing 1h
2.14MPa；Stainless steel and phosphate doped ceramics material are used according to " the natural ornamental stone test methods of GB/T 9966.4-2001 "
Material applies 25N pressure, rotating speed 50rpm/min, abrasion loss 0.29g/cm to mill2。
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (9)
- A kind of 1. phosphate doped ceramics coating material, it is characterised in that：Described phosphate doped ceramics coating material be by Aluminium dihydrogen phosphate-biphosphate chromium solution, diluent and ceramic composition composition, its specific parts by weight composition are as follows：Aluminium dihydrogen phosphate -1~4 part of biphosphate chromium solution15~20 parts of diluent20~40 parts of ceramic composition；Wherein, ceramic composition is made up of the raw material of following parts by weight：
- 2. phosphate doped ceramics coating material as claimed in claim 1, it is characterised in that：Described aluminium dihydrogen phosphate-phosphorus Acid dihydride chromium solution is made up of the raw material of following parts by weight：
- 3. phosphate doped ceramics coating material as claimed in claim 2, it is characterised in that：Described aluminium dihydrogen phosphate-phosphorus The preparation method of acid dihydride chromium solution is as follows：The phosphoric acid solution that mass fraction is 85%, aluminium hydroxide, potassium bichromate or chromium trioxide are weighed according to quality parts ratio, is mixed Conjunction is uniformly mixing to obtain mixed solution, by mixed solution be warming up to 120 DEG C~150 DEG C holding 1h~4h, heating rate be 15 DEG C/ Min~30 DEG C/min, 15 DEG C~25 DEG C are cooled to after the completion of reaction, the hydrogen peroxide or formaldehyde and abundant of formula ratio are added dropwise thereto Stirring, is cooled to 15 DEG C~25 DEG C after being added dropwise to complete, the acetone or alcohol for then adding formula ratio stirs, and obtains di(2-ethylhexyl)phosphate Hydrogen aluminium-biphosphate chromium mixed solution.
- 4. phosphate doped ceramics coating material as claimed in claim 1, it is characterised in that：Described diluent is by following The raw material of parts by weight is made：Mass fraction is 85% 80~120 parts of phosphoric acid solution50~80 parts of distilled water.
- 5. phosphate doped ceramics coating material as claimed in claim 4, it is characterised in that：The preparation side of described diluent Method is as follows：The phosphoric acid solution that mass fraction is 85% is weighed according to quality parts ratio, distilled water, is mixed evenly, is diluted Agent.
- 6. phosphate doped ceramics coating material as claimed in claim 1, it is characterised in that：The particle size range of aluminum oxide is 20 μm~200 μm；The particle size range of aluminium nitride is 200nm~1000nm；The particle size range of silica flour is 5 μm~50 μm；Lithium feldspar The particle size range of powder is 5 μm~50 μm；The particle size range of zirconium oxide is 300nm~1000nm.
- 7. phosphate doped ceramics coating material as claimed in claim 6, it is characterised in that：The preparation of described ceramic composition Method is as follows：By proportioning weigh aluminum oxide, aluminium nitride, zirconium oxide, silica flour, lithium feldspar powder, calcium oxide, magnesia, lead orthoplumbate, Sodium tetraborate and sodium tripolyphosphate, with V-type batch mixer mixing 6h, obtain ceramic composition.
- 8. a kind of method for preparing the phosphate doped ceramics coating material as described in claim any one of 1-7, its feature exist In：The preparation method comprises the following steps that：(1) aluminium dihydrogen phosphate-biphosphate chromium solution is weighed by proportioning, diluent, be mixed evenly, rear addition proportional quantity Ceramic composition, uniform muddy is mixed into, obtains phosphate doped ceramics coating material；(2) the phosphate doped ceramics material that step (1) obtains coated on metal material or can be glued into material surface, controls temperature According to 50 DEG C~150 DEG C, gradient increased temperature, time range is 12h~48h, is molded phosphate doped ceramics material hardening.
- 9. preparation method as claimed in claim 8, it is characterised in that：In step (2), gradient increased temperature requires gradient temperature scope No more than 30 DEG C.
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