GB/T 39530-2020. Thermal spraying-Nanostructured zirconia powder and coating preparation.
1 Scope
GB/T 39530 specifies the chemical and physical properties of nano-zirconia agglomerated powders used in the production of thermal spray coatings, as well as the physical properties of coatings and the technical conditions for coating preparation.
GB/T 39530 is applicable to the production and acceptance of nano-zirconia agglomerated powders for thermal spraying and the acceptance of coatings prepared by thermal spraying nano-zirconia agglomerated powders.
2 Normative references
The following documents are essential for the application of this document. For all dated references, only the dated version applies to this document. For all undated references, the latest version (including all amendments) applies to this document.
GB/T 1479.1 Determination of bulk density of metal powders Part 1: Funnel method
GB/T 1479.2 Determination of bulk density of metal powders Part 2: Scott volumetric method
GB/T 1479.3 Determination of bulk density of metal powders Part 3: Vibrating funnel method
GB/T 1482 Determination of flowability of metal powders Standard funnel method (Hall rheometer)
GB/T 3634.2 Hydrogen Part 2: Pure hydrogen, high purity hydrogen and ultrapure hydrogen
GB/T 4842 Argon
GB/T 4844 Pure helium, high purity helium and ultrapure helium
GB/T 8642 Determination of tensile bond strength of thermal spraying
GB/T 8979 Pure nitrogen, high purity nitrogen and ultra-pure nitrogen
GB/T 11373 Surface pretreatment of thermal sprayed metal parts
GB/T 11374 Non-destructive measurement method for thickness of thermal sprayed coatings
GB/T 19356 Composition and technical supply conditions
of thermal spraying powders GB/T 23413 Determination of grain size and micro-strain of nanomaterials by X-ray diffraction line broadening method
GB/T 31568 Determination of grain size of thermal sprayed thermal barrier ZrO2 coatings by Scherrer formula method
GB/T 37421 Thermal spraying Characterization and testing of thermal sprayed coatings
ISO 13123 Metallic and other inorganic coatings-Test method of cyclic heating for thermal-barrier coatings under temperature gradient
This standard specifies the chemical and physical properties of nano-zirconia agglomerated powders used in the production of thermal spray coatings, the physical properties of coatings, and the technical conditions for coating preparation. This standard applies to the production and acceptance of nano-zirconia agglomerated powders for thermal spraying and the acceptance of coatings prepared from nano-zirconia agglomerated powders for thermal spraying.

ICS25.220.20
National Standard of the People's Republic of China
GB/T39530—2020
Thermal spraying
Nanostructured zirconia powder and coating preparation
Technical conditions
Thermal sprayingNanostructured zirconia powder and coating preparation2020-12-14ReleasebZxz.net
State Administration for Market Regulation
National Administration of Standardization
Release
2021-11-01Implementation
GB/T39530—2020
Foreword
Scope
Normative references
Technical requirements
Nanostructured zirconia powder
Nanostructured zirconia powder spraying Technology
Requirements for nano-zirconia powder spray coating
4 Inspection method
Thermal spraying of nano-zirconia agglomerated powder
Nano-zirconia powder spray coating
5 Marking, packaging, transportation and storage
Marking
Packaging
Transportation
Storage
Foreword
This standard is drafted in accordance with the rules given in GB/T1.1-2009. This standard is proposed by the China Machinery Industry Federation. This standard is under the jurisdiction of the National Technical Committee for Standardization of Metallic and Non-metallic Coverings (SAC/TC57). GB/T39530—2020
Drafting units of this standard: Wuhan Institute of Materials Protection Co., Ltd., Aerospace Materials and Technology Research Institute, Shanghai Informan Nanotechnology Co., Ltd., Beijing Jinlun Kuntian Special Machinery Co., Ltd., Beijing Mining and Metallurgical Technology Group Co., Ltd., Jiangsu Zhongkuang Dazheng Surface Engineering Technology Co., Ltd.
The main drafters of this standard: Wu Jianhua, Wu Chaojun, He Deng, Li Gang, Yu Yueguang, Chen Tongzhou, Ni Liyong, Zou Han, Tian Qingfen, Shen Jie, Yi Juan, Kang Zhuangsu, Fang Erbao.
1 Scope
Thermal spraying
Nano oxide powder and coating preparation
Technical conditions
GB/T39530—2020
This standard specifies the chemical and physical properties of nano zirconium oxide agglomerated powders used to produce thermal spray coatings, as well as the physical properties of coatings and the technical conditions for coating preparation
This standard applies to the production and acceptance of nano zirconium oxide agglomerated powders for thermal spraying and the acceptance of coatings prepared by thermal spraying nano zirconium oxide agglomerated powders.
Normative referenced documents
The following documents are indispensable for the application of this document. For all dated referenced documents, only the dated version applies to this document. For any undated referenced document, the latest version (including all amendments) shall apply to this document. GB/T 1479.1 Determination of bulk density of metal powders Part 1: Funnel method GB/T 1479.2 GB/T 1479.3 Determination of bulk density of metal powders Part 1: Funnel method 1479.3
GB/T1482
Determination of bulk density of metal powders Part 2: Scott volumetric methodDetermination of bulk density of metal powders Part 3: Vibrating funnel methodDetermination of flowability of metal powders Standard funnel method (Hall rheometer)GB/T3634.2
Hydrogen Part 2: Pure hydrogen, high purity hydrogen and ultrapure hydrogen and fluorine
GB/T4842
GB/T-4844
GB/T8642
GB/T8979
GB/T11373
Pure ammonia, high purity ammonia and ultrapure ammonia
Determination of tensile bond strength of thermal spraying
Pure nitrogen, high purity nitrogen and ultrapure nitrogen Pure nitrogen
Pretreatment of the surface of thermal sprayed metal partsGB/T11374
GB/T19356
GB/T23413
GB/T31568
Non-destructive measurement method of thermal spray coating thicknessComposition and supply technical conditions of thermal spray powderDetermination of grain size and micro-strain of nanomaterialsX-ray diffraction line broadening methodDetermination of grain size of thermal barrier ZrO2 coatings by thermal sprayingScherrer formula methodGB/T37421
Thermal sprayCharacterization and testing of thermal spray coatingsISO13123Method for thermal cycling test of thermal barrier coatings under temperature gradient for metallic and other inorganic covering layers (Metallic and other inorganic covering layers) ISO13826Metallic and other inorganic coatingsDetermination of thermal diffusivity of thermally sprayed ceramic coatingsby laser flash method)
ISO14188Metallic and other inorganic coatingsTest methods for measuring thermal cycle resistance and thermal shock resistanceforthermal barrier coatings)
ISO18332Metallic and other inorganic coatings—Definitions and conventions concerning porosity porosity1
GB/T39530—2020
ISO18555Metallic and other inorganic coatingsDetermination of thermal conductivity of thermal barrier coatingsISO19477Metallic and other inorganic coatingsMeasurement of Young's modulus of thermal barrier coatings by beam deflection bending)ISO/TR26946 Determination of porosity of thermally sprayed coatings (Standard method for porosity measurement of thermally sprayed coatings)
3 Technical requirements
Nano zirconia powder
3.1.1
Material selection
Thermal spraying nano zirconia powder does not select nano zirconia powder prepared by co-precipitation method, hydrothermal method and other processes as raw material, with a grain size of 100nm. The material composition is shown in Table 1.
Table 1
Composition of nano-zirconia powder
Serial number
ZrO,+HfO
94.6±0.4
92.0±1.0
86.4±0.4
5.2±0.4
8.0±1.0
13.3±0.4
Sio,
0.02
0.02
0.02
Fe20
Mass fraction/%
0.05
0.05
0.05
The composition of nano-zirconia powder can also be determined according to user requirements. 3.1.2 Preparation process
0.02
0.02
≤0.02
Naz0
0.02
0.02
0.02
Mg：0
0.02
0.02
0.02
0.02
≤0.02
0.02
TiO.
0.02
0.02
0.02
0.03
≤0.03
0.03
The thermal sprayed nano-zirconia agglomerated powder is obtained by spray drying agglomeration, heat treatment and densification. Usually a heating furnace is used for heat treatment and densification, the treatment temperature is 900℃1400℃, and the insulation time is 0.5h～24h. Plasma or arc spheroidization densification treatment can also be used according to user requirements.
3.1.3 Thermal sprayed nano-zirconia agglomerated powder particle size The typical particle size range of thermal sprayed nano-zirconia agglomerated powder should be suitable for plasma spraying process. The typical particle size range of thermal spraying nano-zirconia agglomerated powder is: <30μm;
15μm~45μm;
15μm~90μm;
45μm~90μm.
Or determine the particle size range and particle size distribution according to user requirements. 3.1.4 Loose density of thermal spraying nano-zirconia agglomerated powder The loose density of thermal spraying nano-zirconia agglomerated powder is: 1.5g/cm ≤ p ≤ 2.3g/cm. The loose density of thermal spraying nano-zirconia agglomerated powder can also be determined by negotiation among the relevant parties. 2
3.1.5 Fluidity of thermal sprayed nano-zirconia agglomerated powder GB/T39530—2020
The morphology of thermal sprayed nano-zirconia agglomerated powder should be spherical or approximately spherical. The fluidity of 15μm~90μm and 45μm~90μm thermal sprayed nano-zirconia agglomerated powder after heat treatment and densification is less than or equal to 80s/50g, and the fluidity of 15uμm~45um thermal sprayed nano-zirconia agglomerated powder is less than or equal to 100s/50g. The fluidity of 15μm~90μm and 45um90μm thermal sprayed nano-zirconia agglomerated powder treated with plasma or arc spheroidization is less than or equal to 50s/50g, and the fluidity of 15μm~45μm thermal sprayed nano-zirconia agglomerated powder is less than or equal to 80s/50g. The fluidity of thermal sprayed nano-zirconia agglomerated powder can also be determined by negotiation among the relevant parties. 3.2 Nano-zirconia powder spraying process
3.2.1 Surface pretreatment
The parts to be sprayed should be surface pretreated in accordance with GB/T11373, and the time interval from the end of pretreatment to the start of spraying should be less than or equal to 4h3.2.2 Powder drying
Before spraying, the spraying powder should be dried for more than 1h in the temperature range of 100℃～120℃. The powder accumulation thickness is less than or equal to 30mm
3.2.3 Spraying process
Nano-zirconia powder should not be sprayed by plasma spraying process, including atmospheric plasma spraying, vacuum plasma spraying, etc.3.2.4 Spraying gas
Nitrogen used for plasma spraying should meet the requirements of GB/T8979, and the purity should be greater than 99.99%. Argon should meet the requirements of GB/T4842, and the purity should be greater than 99.99%. Hydrogen should meet the requirements of GB/T3634.2, with a purity greater than 99.99%. Ammonia should meet the requirements of GB/T4844, with a purity greater than 99.99%.
3.2.5 Preheating
Before spraying, the surface of the substrate should be preheated. The spray gun can be used for preheating, or other methods can be used. The preheating temperature should be determined according to the substrate material.
3.2.6 Spraying the bonding coating
After the sprayed parts are preheated, the powder is immediately sent to spray the bonding coating. The bonding coating can be sprayed by high-speed flame spraying, vacuum plasma spraying and atmospheric plasma spraying.
The bonding coating material should meet the requirements of relevant technical standards. The bonding coating thickness should meet the requirements of the design drawings. 3.2.7 Spraying the nano-zirconia coating
After spraying the bonding coating, the nano-zirconia coating should be sprayed within 2 hours, and the spraying should be carried out continuously. The coating thickness should meet the design requirements. 3.3 Requirements for Nano Zirconia Powder Spray Coating 3.3.1 Appearance
The spraying parts specified in the design drawing shall be fully covered with coating, and the non-spraying parts shall be shielded and protected. The coating shall be complete, the surface shall be even and continuous, and there shall be no visible defects such as cracks, peeling, bulging and edge lifting. GB/T39530—2020
3.3.2 Thickness
The coating thickness shall comply with the requirements of the design drawing and relevant technical documents. The total coating thickness (combined coating ten-sided layer) is generally 0.35mm~0.50mm or meets the requirements of the design drawing. 3.3.3 Bonding Strength
The bonding strength of the nano zirconium oxide powder spray coating and the bonding coating shall be greater than or equal to 30MPa or meet the requirements of the design drawing. 3.3.4 Thermal Shock Performance
The nano zirconium oxide powder spray coating shall be subjected to thermal shock test assessment according to the standard. The thermal shock conditions, thermal shock test temperature and thermal shock times can be determined by negotiation among the relevant parties. 3.3.5 Microstructure
3.3.5.1 General requirements
The microstructure of nano-zirconia powder spray coating should be uniform, without delamination and separation between the coating and the substrate. 3.3.5.2 Interface state
When measured by metallographic method, the interface holes between the metal substrate and the bonding coating and the bonding coating and the nano-zirconia powder spray coating are less than or equal to 10%, and the interface pollutants (including oxides/sand particles) are less than or equal to 30%. 3.3.5.3 Porosity
The porosity and pore diameter of the nano-zirconia powder spray coating should meet the design requirements. 3.3.6 Other requirements
Other requirements of nano-zirconia powder spray coating, such as the unmelted particles, thermal diffusivity, thermal conductivity, Young's modulus, etc. of the coating, can be determined by negotiation among the relevant parties.
4: Test method
4.1 Thermal sprayed nano-zirconia agglomerated powder
4.1.1 Chemical composition
The chemical composition of thermal sprayed nano-zirconia agglomerated powder can be determined by various appropriate methods, such as: ICP-OES coupling method (inductively coupled plasma emission spectrometry), wet chemical method, etc. 4.1.2 Powder particle size range
The particle size distribution (PSD) of thermal sprayed nano-zirconia agglomerated powder can be determined by screening method, airflow screening method, laser scattering method and other methods.
When using the screening method (applicable powder particle size range is 125um~38um), the maximum weight of the powder with particles larger than the specified upper limit size and smaller than the specified lower limit size is 10%.
When using the airflow screening method (applicable powder particle size range is 45μm~5um), the maximum weight of the powder with particles larger than the specified upper limit size is 5%, and the maximum weight of the powder with particles smaller than the specified lower limit size is 10%. When using the laser scattering method (applicable powder size range is 63um~5um), the weight of the powder with particles larger than the specified upper limit size is 4
25% at most, and the weight of the powder with particles smaller than the specified lower limit size is 5% at most. 4.1.3 Bulk density
GB/T39530—2020
The bulk density of thermal sprayed nano-zirconia agglomerated powder shall be determined in accordance with the provisions of GB/T1479.1 or GB/T1479.2 or GB/T1479.3.
4.1.4 Powder fluidity
The fluidity of thermal sprayed nano-zirconia agglomerated powder shall be determined in accordance with the provisions of GB/T1482. 4.1.5 Powder morphology
The morphology of thermal sprayed nano-zirconia agglomerated powder shall be observed by scanning electron microscope and stereo microscope in accordance with the provisions of GB/T19356. 4.1.6 Grain size
The grain size of nano-zirconia before heat treatment or spheroidization can be determined by scanning electron microscope, etc., or by X-ray diffraction line broadening method in accordance with the provisions of GB/T23413. The grain size of thermal sprayed nano-zirconia agglomerated powder after heat treatment or spheroidization shall be determined in accordance with the provisions of GB/T23413. 4.2 Nano-zirconia powder spray coating
4.2.1 Appearance
Visually inspect the coating appearance under natural light or non-reflected light. The illumination should not be less than 3001x (equivalent to the illumination of the part at 0.5m under a 40W fluorescent lamp). If necessary, a 5-10x magnifying glass can be used for inspection. 4.2.2 Coating thickness
4.2.2.1 General
The coating thickness can be measured on the part or on the furnace-mounted part. The specific measurement method shall be specified in the process specification according to the part, or determined by negotiation among the relevant parties.
4.2.2.2 Measurement with general measuring tools or metallographic method
The coating thickness is measured with general measuring tools such as micrometer (the measurement accuracy should be not less than 0.02mm) or metallographic method. 4.2.2.3 Thickness gauge measurement
When the substrate is a magnetic metal material, the thickness of the non-magnetic material combined coating and the unsprayed coating of nano-zirconia powder can be measured with a magnetic thickness gauge in accordance with the provisions of GB/T11374.
The nano-zirconia powder sprayed coating on the metal substrate can also be measured with an eddy current thickness gauge. 4.2.3 Coating porosity
The porosity of nano-zirconia powder spray coatings shall be determined in accordance with ISO18332 or ISO/TR26946. 4.2.4 Coating bonding strength
The bonding strength of nano-zirconia powder spray coatings shall be determined in accordance with GB/T8642. Coatings with a porosity higher than 5% shall use solid film glue, and the tensile loading rate shall be less than or equal to 1mm/min. 5
GB/T39530—2020
4.2.5 Microstructure
Use a 500x metallographic microscope to check for cracks in the coating, a 500x metallographic microscope to check for cracks and unmelted particles in the coating, and a 200x metallographic microscope to check for interface contamination and interface holes between the coating and the substrate. 4.2.6 Thermal shock properties of coatings
The thermal shock properties of nano-zirconia powder sprayed coatings shall be measured in accordance with ISO14188 when heated by a high-temperature furnace, water-cooled or air-cooled; when heated by gas, they shall be measured in accordance with ISO13123. 4.2.7 Grain size of coatings
The grain size of nano-zirconia powder unsprayed coatings may be measured in accordance with GB/T31568. 4.2.8 Thermal diffusivity of coatings
The thermal diffusivity of nano-zirconia powder sprayed coatings shall be measured in accordance with ISO13826. 4.2.9 Thermal conductivity of coatings
The thermal conductivity of nano-zirconia powder sprayed coatings shall be measured in accordance with ISO18555. 4.2.10 Young's modulus of coatings
Young's modulus of nano-zirconia powder unsprayed coatings shall be measured in accordance with ISO19477. 4.2.11 Others
Other characteristics of nano-oxidation powder spray coatings can be tested in accordance with the provisions of GB/T37421. Note: 4.2.1~4.2.5 are mandatory inspection items, and others are negotiated inspection items. 5 Marking, packaging, transportation and storage
5.1 Marking
The product packaging should clearly indicate the product name, powder composition, particle size range, quantity, powder batch, production date, standard number, factory name, and attach a product certificate.
2 Packaging
Powders should be packed in moisture-proof sealed containers. Special packaging shall be agreed upon by the supply and demand parties. 5.3
Transportation
During transportation, attention should be paid to rain and moisture protection. 5.4 Purchase and storage
Powders should be stored in ventilated, dry and clean rooms. 6
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