熱分解法は、仲タングステン酸アンモニウム（APT）を原料として使用し、高温処理によって直接偏タングステン酸アンモニウム（AMT）を製造します。プロセスの流れは以下の通りです：
- 加熱分解: APTを200-300℃の環境に置き、部分的に分解させ、アンモニアガス（NH₃）と水蒸気を放出させます。
- 溶液処理: 分解生成物を水に溶解し、pHを調整してAMTを生成します。
- 結晶分離: 溶液を濃縮し、冷却して結晶化させ、乾燥して製品を得ます。
反応プロセスは大まかに次のように表すことができます：
この方法は簡単ですが、制御が難しいです。温度が高すぎると、WO₃が直接生成され、収率が低下します。したがって、熱分解法は主に実験室の研究や小規模な生産に使用され、産業用途は限られています。
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